# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2018

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1831436'
_audit_update_record             
;
2018-03-21 deposited with the CCDC.
2018-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        datolite
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B Ca H O5 Si'
_chemical_formula_weight         159.99

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0522 0.0431 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0004 0.0004 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.1611 0.1926 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   4.787(3)
_cell_length_b                   7.5640(3)
_cell_length_c                   9.6012(5)
_cell_angle_alpha                90
_cell_angle_beta                 90.283(13)
_cell_angle_gamma                90
_cell_volume                     347.68(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1660
_cell_measurement_theta_min      2.047
_cell_measurement_theta_max      17.429

_exptl_crystal_description       isosymmetric
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    3.056
_exptl_crystal_F_000             320
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.010
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.005
_exptl_absorpt_coefficient_mu    1.041
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.2896
_diffrn_radiation_type           ?
_diffrn_source                   ?
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            1660
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.047
_diffrn_reflns_theta_max         17.429
_diffrn_reflns_theta_full        10.007
_diffrn_measured_fraction_theta_max 0.262
_diffrn_measured_fraction_theta_full 0.431
_diffrn_reflns_Laue_measured_fraction_max 0.262
_diffrn_reflns_Laue_measured_fraction_full 0.431
_diffrn_reflns_point_group_measured_fraction_max 0.262
_diffrn_reflns_point_group_measured_fraction_full 0.431
_reflns_number_total             842
_reflns_number_gt                737
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0351P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.08(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         842
_refine_ls_number_parameters     78
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0290
_refine_ls_wR_factor_ref         0.0795
_refine_ls_wR_factor_gt          0.0772
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.0072(2) 0.60649(4) 0.16461(4) 0.0064(4) Uani 1 1 d . . . . .
Si1 Si 0.4717(3) 0.26743(6) 0.08421(5) 0.0048(6) Uani 1 1 d . . . . .
B1 B 0.5683(14) 0.0891(2) -0.1587(2) 0.005(3) Uani 1 1 d . . . . .
O1 O 0.2429(9) 0.40374(15) 0.03637(14) 0.0075(16) Uani 1 1 d . . . . .
O2 O 0.6750(8) 0.19836(15) -0.04188(13) 0.0051(16) Uani 1 1 d . . . . .
O3 O 0.6794(8) 0.33507(16) 0.21107(12) 0.0045(15) Uani 1 1 d . . . . .
O4 O 0.3126(8) 0.08946(15) 0.14543(14) 0.0070(16) Uani 1 1 d . . . . .
O5 O 0.2594(10) 0.08784(17) -0.16322(15) 0.006(2) Uani 1 1 d D . . . .
H H 0.193(13) 0.045(4) -0.086(3) 0.021(10) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O1 2.267(2) 3_565 ?
Ca1 O1 2.270(3) . ?
Ca1 O4 2.391(3) 2 ?
Ca1 O2 2.429(3) 3_665 ?
Ca1 O5 2.516(2) 4_566 ?
Ca1 O3 2.578(2) 2_655 ?
Ca1 O3 2.624(3) 1_455 ?
Ca1 O5 2.641(3) 3_565 ?
Ca1 B1 3.071(5) 3_665 ?
Ca1 B1 3.085(5) 4_466 ?
Ca1 Si1 3.4379(14) 3_565 ?
Ca1 Si1 3.4834(15) . ?
Si1 O1 1.571(3) . ?
Si1 O2 1.642(3) . ?
Si1 O3 1.650(2) . ?
Si1 O4 1.656(2) . ?
Si1 Ca1 3.4379(14) 3_565 ?
Si1 Ca1 3.5510(16) 2_545 ?
Si1 Ca1 3.5914(17) 3_665 ?
B1 O4 1.472(3) 3_655 ?
B1 O3 1.477(4) 4_565 ?
B1 O5 1.480(7) . ?
B1 O2 1.482(3) . ?
B1 Ca1 3.071(5) 3_665 ?
B1 Ca1 3.085(5) 4_665 ?
O1 Ca1 2.267(2) 3_565 ?
O2 Ca1 2.429(3) 3_665 ?
O3 B1 1.477(4) 4_566 ?
O3 Ca1 2.578(2) 2_645 ?
O3 Ca1 2.624(3) 1_655 ?
O4 B1 1.472(3) 3_655 ?
O4 Ca1 2.391(3) 2_545 ?
O5 Ca1 2.516(2) 4_565 ?
O5 Ca1 2.641(3) 3_565 ?
O5 H 0.87(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ca1 O1 77.12(13) 3_565 . ?
O1 Ca1 O4 108.05(13) 3_565 2 ?
O1 Ca1 O4 134.36(7) . 2 ?
O1 Ca1 O2 86.41(10) 3_565 3_665 ?
O1 Ca1 O2 80.41(9) . 3_665 ?
O4 Ca1 O2 143.90(5) 2 3_665 ?
O1 Ca1 O5 142.08(5) 3_565 4_566 ?
O1 Ca1 O5 73.95(7) . 4_566 ?
O4 Ca1 O5 76.96(11) 2 4_566 ?
O2 Ca1 O5 111.97(14) 3_665 4_566 ?
O1 Ca1 O3 136.10(5) 3_565 2_655 ?
O1 Ca1 O3 114.49(12) . 2_655 ?
O4 Ca1 O3 93.23(8) 2 2_655 ?
O2 Ca1 O3 56.81(6) 3_665 2_655 ?
O5 Ca1 O3 79.13(7) 4_566 2_655 ?
O1 Ca1 O3 78.71(8) 3_565 1_455 ?
O1 Ca1 O3 82.12(10) . 1_455 ?
O4 Ca1 O3 56.10(6) 2 1_455 ?
O2 Ca1 O3 159.17(5) 3_665 1_455 ?
O5 Ca1 O3 73.54(10) 4_566 1_455 ?
O3 Ca1 O3 142.49(4) 2_655 1_455 ?
O1 Ca1 O5 76.84(7) 3_565 3_565 ?
O1 Ca1 O5 146.11(5) . 3_565 ?
O4 Ca1 O5 74.91(8) 2 3_565 ?
O2 Ca1 O5 76.67(12) 3_665 3_565 ?
O5 Ca1 O5 138.16(4) 4_566 3_565 ?
O3 Ca1 O5 72.26(10) 2_655 3_565 ?
O3 Ca1 O5 113.35(12) 1_455 3_565 ?
O1 Ca1 B1 110.89(8) 3_565 3_665 ?
O1 Ca1 B1 99.55(13) . 3_665 ?
O4 Ca1 B1 118.73(8) 2 3_665 ?
O2 Ca1 B1 28.30(5) 3_665 3_665 ?
O5 Ca1 B1 97.74(10) 4_566 3_665 ?
O3 Ca1 B1 28.64(6) 2_655 3_665 ?
O3 Ca1 B1 170.40(6) 1_455 3_665 ?
O5 Ca1 B1 70.34(12) 3_565 3_665 ?
O1 Ca1 B1 95.36(12) 3_565 4_466 ?
O1 Ca1 B1 108.41(9) . 4_466 ?
O4 Ca1 B1 27.64(5) 2 4_466 ?
O2 Ca1 B1 171.19(8) 3_665 4_466 ?
O5 Ca1 B1 71.60(12) 4_566 4_466 ?
O3 Ca1 B1 117.61(7) 2_655 4_466 ?
O3 Ca1 B1 28.55(6) 1_455 4_466 ?
O5 Ca1 B1 95.29(11) 3_565 4_466 ?
B1 Ca1 B1 145.30(6) 3_665 4_466 ?
O1 Ca1 Si1 21.64(6) 3_565 3_565 ?
O1 Ca1 Si1 98.16(6) . 3_565 ?
O4 Ca1 Si1 96.75(8) 2 3_565 ?
O2 Ca1 Si1 84.92(7) 3_665 3_565 ?
O5 Ca1 Si1 159.19(7) 4_566 3_565 ?
O3 Ca1 Si1 121.35(4) 2_655 3_565 ?
O3 Ca1 Si1 86.43(6) 1_455 3_565 ?
O5 Ca1 Si1 55.46(5) 3_565 3_565 ?
B1 Ca1 Si1 102.61(7) 3_665 3_565 ?
B1 Ca1 Si1 93.52(9) 4_466 3_565 ?
O1 Ca1 Si1 96.97(7) 3_565 . ?
O1 Ca1 Si1 20.45(5) . . ?
O4 Ca1 Si1 122.77(5) 2 . ?
O2 Ca1 Si1 86.44(8) 3_665 . ?
O5 Ca1 Si1 53.90(6) 4_566 . ?
O3 Ca1 Si1 103.05(8) 2_655 . ?
O3 Ca1 Si1 81.06(7) 1_455 . ?
O5 Ca1 Si1 162.26(8) 3_565 . ?
B1 Ca1 Si1 97.16(11) 3_665 . ?
B1 Ca1 Si1 101.88(8) 4_466 . ?
Si1 Ca1 Si1 118.33(3) 3_565 . ?
O1 Si1 O2 114.09(11) . . ?
O1 Si1 O3 115.41(10) . . ?
O2 Si1 O3 106.59(18) . . ?
O1 Si1 O4 108.42(19) . . ?
O2 Si1 O4 106.16(11) . . ?
O3 Si1 O4 105.46(10) . . ?
O1 Si1 Ca1 32.14(5) . 3_565 ?
O2 Si1 Ca1 88.38(10) . 3_565 ?
O3 Si1 Ca1 145.53(6) . 3_565 ?
O4 Si1 Ca1 99.55(11) . 3_565 ?
O1 Si1 Ca1 30.33(6) . . ?
O2 Si1 Ca1 141.15(6) . . ?
O3 Si1 Ca1 89.50(10) . . ?
O4 Si1 Ca1 102.98(13) . . ?
Ca1 Si1 Ca1 61.67(3) 3_565 . ?
O1 Si1 Ca1 88.39(13) . 2_545 ?
O2 Si1 Ca1 141.13(6) . 2_545 ?
O3 Si1 Ca1 89.64(11) . 2_545 ?
O4 Si1 Ca1 34.98(9) . 2_545 ?
Ca1 Si1 Ca1 97.84(5) 3_565 2_545 ?
Ca1 Si1 Ca1 71.75(3) . 2_545 ?
O1 Si1 Ca1 96.71(12) . 3_665 ?
O2 Si1 Ca1 34.72(7) . 3_665 ?
O3 Si1 Ca1 89.46(12) . 3_665 ?
O4 Si1 Ca1 140.73(10) . 3_665 ?
Ca1 Si1 Ca1 85.83(3) 3_565 3_665 ?
Ca1 Si1 Ca1 113.46(3) . 3_665 ?
Ca1 Si1 Ca1 174.70(3) 2_545 3_665 ?
O4 B1 O3 106.8(3) 3_655 4_565 ?
O4 B1 O5 112.5(3) 3_655 . ?
O3 B1 O5 110.0(3) 4_565 . ?
O4 B1 O2 108.3(3) 3_655 . ?
O3 B1 O2 107.5(3) 4_565 . ?
O5 B1 O2 111.5(3) . . ?
O4 B1 Ca1 115.7(4) 3_655 3_665 ?
O3 B1 Ca1 56.80(17) 4_565 3_665 ?
O5 B1 Ca1 131.74(13) . 3_665 ?
O2 B1 Ca1 50.99(19) . 3_665 ?
O4 B1 Ca1 48.91(19) 3_655 4_665 ?
O3 B1 Ca1 58.10(19) 4_565 4_665 ?
O5 B1 Ca1 131.62(13) . 4_665 ?
O2 B1 Ca1 116.8(4) . 4_665 ?
Ca1 B1 Ca1 84.09(16) 3_665 4_665 ?
Si1 O1 Ca1 126.22(8) . 3_565 ?
Si1 O1 Ca1 129.22(7) . . ?
Ca1 O1 Ca1 102.88(13) 3_565 . ?
B1 O2 Si1 122.1(4) . . ?
B1 O2 Ca1 100.7(2) . 3_665 ?
Si1 O2 Ca1 122.63(7) . 3_665 ?
B1 O3 Si1 121.8(3) 4_566 . ?
B1 O3 Ca1 94.56(15) 4_566 2_645 ?
Si1 O3 Ca1 118.76(7) . 2_645 ?
B1 O3 Ca1 93.35(17) 4_566 1_655 ?
Si1 O3 Ca1 118.42(7) . 1_655 ?
Ca1 O3 Ca1 104.85(12) 2_645 1_655 ?
B1 O4 Si1 126.8(3) 3_655 . ?
B1 O4 Ca1 103.5(2) 3_655 2_545 ?
Si1 O4 Ca1 121.63(9) . 2_545 ?
B1 O5 Ca1 119.96(16) . 4_565 ?
B1 O5 Ca1 118.52(12) . 3_565 ?
Ca1 O5 Ca1 106.13(13) 4_565 3_565 ?
B1 O5 H 110(4) . . ?
Ca1 O5 H 99(3) 4_565 . ?
Ca1 O5 H 99(3) 3_565 . ?

_refine_diff_density_max         0.446
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.125



# start Validation Reply Form
_vrf_PLAT029_shelx               
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.431 Why?  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT051_shelx               
;
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by .      81.70 %     
RESPONSE: ...
;
_vrf_PLAT031_shelx               
;
PROBLEM: Refined Extinction Parameter Within Range ......      1.333 Sigma 
RESPONSE: ...
;
_vrf_PLAT911_shelx               
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        317 Report
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT927_shelx               
;
PROBLEM: Reported and Calculated  wR2 Differ by .........    -0.0054 Check 
RESPONSE: ...
;
# end Validation Reply Form

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1831439'
_audit_update_record             
;
2018-03-21 deposited with the CCDC.
2018-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B Ca H O5 Si'
_chemical_formula_weight         159.99

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0522 0.0431 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0004 0.0004 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.1611 0.1926 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   4.526(4)
_cell_length_b                   7.2220(4)
_cell_length_c                   9.3443(3)
_cell_angle_alpha                90
_cell_angle_beta                 91.080(13)
_cell_angle_gamma                90
_cell_volume                     305.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1087
_cell_measurement_theta_min      1.452
_cell_measurement_theta_max      17.235

_exptl_crystal_description       isosymmetric
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.479
_exptl_crystal_F_000             320
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.010
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.005
_exptl_absorpt_coefficient_mu    1.185
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.2896
_diffrn_radiation_type           ?
_diffrn_source                   ?
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            1087
_diffrn_reflns_av_unetI/netI     0.0703
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_h_max       2
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.452
_diffrn_reflns_theta_max         17.235
_diffrn_reflns_theta_full        10.007
_diffrn_measured_fraction_theta_max 0.176
_diffrn_measured_fraction_theta_full 0.330
_diffrn_reflns_Laue_measured_fraction_max 0.176
_diffrn_reflns_Laue_measured_fraction_full 0.330
_diffrn_reflns_point_group_measured_fraction_max 0.176
_diffrn_reflns_point_group_measured_fraction_full 0.330
_reflns_number_total             482
_reflns_number_gt                395
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0871P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         482
_refine_ls_number_parameters     77
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0520
_refine_ls_wR_factor_ref         0.1350
_refine_ls_wR_factor_gt          0.1225
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_restrained_S_all      0.978
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.0048(6) 0.61006(10) 0.16960(6) 0.033(2) Uani 1 1 d . . . . .
Si1 Si 0.4871(10) 0.27955(15) 0.08120(9) 0.036(3) Uani 1 1 d . . . . .
B1 B 0.593(9) 0.0824(8) -0.1552(9) 0.03(2) Uani 1 1 d . . . . .
O1 O 0.253(2) 0.4221(4) 0.0307(3) 0.029(7) Uani 1 1 d . . . . .
O2 O 0.702(3) 0.1929(4) -0.0373(2) 0.029(6) Uani 1 1 d . . . . .
O3 O 0.704(2) 0.3409(4) 0.2136(2) 0.035(6) Uani 1 1 d . . . . .
O4 O 0.305(3) 0.1007(4) 0.1403(3) 0.030(7) Uani 1 1 d . . . . .
O5 O 0.262(6) 0.0902(7) -0.1614(7) 0.022(14) Uani 1 1 d D . . . .
H H 0.093(15) 0.056(11) -0.119(10) 0.06(4) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O1 2.198(6) 3_565 ?
Ca1 O1 2.200(7) . ?
Ca1 O4 2.285(8) 2 ?
Ca1 O2 2.318(7) 3_665 ?
Ca1 O3 2.377(6) 2_655 ?
Ca1 O3 2.412(7) 1_455 ?
Ca1 O5 2.424(12) 4_566 ?
Ca1 O5 2.481(13) 3_565 ?
Ca1 B1 2.86(3) 4_466 ?
Ca1 B1 2.88(3) 3_665 ?
Ca1 Si1 3.300(4) 3_565 ?
Ca1 Si1 3.349(4) . ?
Si1 O1 1.546(9) . ?
Si1 O2 1.614(8) . ?
Si1 O3 1.627(7) . ?
Si1 O4 1.634(7) . ?
Si1 Ca1 3.300(4) 3_565 ?
Si1 Ca1 3.409(4) 3_665 ?
Si1 Ca1 3.435(4) 1_655 ?
Si1 Ca1 3.465(4) 2_645 ?
Si1 Ca1 3.475(4) 2_545 ?
B1 O4 1.406(14) 3_655 ?
B1 O2 1.441(12) . ?
B1 O3 1.45(2) 4_565 ?
B1 O5 1.50(5) . ?
B1 Ca1 2.86(3) 4_665 ?
B1 Ca1 2.88(3) 3_665 ?
O1 Ca1 2.198(6) 3_565 ?
O2 Ca1 2.318(7) 3_665 ?
O3 B1 1.45(2) 4_566 ?
O3 Ca1 2.377(6) 2_645 ?
O3 Ca1 2.412(7) 1_655 ?
O4 B1 1.407(14) 3_655 ?
O4 Ca1 2.285(8) 2_545 ?
O5 Ca1 2.424(12) 4_565 ?
O5 Ca1 2.481(13) 3_565 ?
O5 H 0.90(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ca1 O1 72.6(4) 3_565 . ?
O1 Ca1 O4 109.6(4) 3_565 2 ?
O1 Ca1 O4 140.14(15) . 2 ?
O1 Ca1 O2 84.8(3) 3_565 3_665 ?
O1 Ca1 O2 76.2(2) . 3_665 ?
O4 Ca1 O2 142.99(13) 2 3_665 ?
O1 Ca1 O3 138.17(13) 3_565 2_655 ?
O1 Ca1 O3 114.8(4) . 2_655 ?
O4 Ca1 O3 90.4(2) 2 2_655 ?
O2 Ca1 O3 59.81(15) 3_665 2_655 ?
O1 Ca1 O3 76.6(2) 3_565 1_455 ?
O1 Ca1 O3 84.2(3) . 1_455 ?
O4 Ca1 O3 59.16(17) 2 1_455 ?
O2 Ca1 O3 156.28(10) 3_665 1_455 ?
O3 Ca1 O3 142.76(10) 2_655 1_455 ?
O1 Ca1 O5 137.10(17) 3_565 4_566 ?
O1 Ca1 O5 76.8(4) . 4_566 ?
O4 Ca1 O5 76.8(6) 2 4_566 ?
O2 Ca1 O5 116.2(7) 3_665 4_566 ?
O3 Ca1 O5 82.2(3) 2_655 4_566 ?
O3 Ca1 O5 71.0(5) 1_455 4_566 ?
O1 Ca1 O5 79.4(3) 3_565 3_565 ?
O1 Ca1 O5 140.7(3) . 3_565 ?
O4 Ca1 O5 75.1(5) 2 3_565 ?
O2 Ca1 O5 74.4(6) 3_665 3_565 ?
O3 Ca1 O5 70.6(5) 2_655 3_565 ?
O3 Ca1 O5 115.6(7) 1_455 3_565 ?
O5 Ca1 O5 140.3(2) 4_566 3_565 ?
O1 Ca1 B1 95.4(5) 3_565 4_466 ?
O1 Ca1 B1 112.5(4) . 4_466 ?
O4 Ca1 B1 29.0(2) 2 4_466 ?
O2 Ca1 B1 171.0(5) 3_665 4_466 ?
O3 Ca1 B1 116.0(2) 2_655 4_466 ?
O3 Ca1 B1 30.27(19) 1_455 4_466 ?
O5 Ca1 B1 69.4(9) 4_566 4_466 ?
O5 Ca1 B1 96.8(9) 3_565 4_466 ?
O1 Ca1 B1 111.6(2) 3_565 3_665 ?
O1 Ca1 B1 96.8(6) . 3_665 ?
O4 Ca1 B1 117.2(4) 2 3_665 ?
O2 Ca1 B1 29.8(2) 3_665 3_665 ?
O3 Ca1 B1 30.1(2) 2_655 3_665 ?
O3 Ca1 B1 171.7(3) 1_455 3_665 ?
O5 Ca1 B1 101.2(6) 4_566 3_665 ?
O5 Ca1 B1 68.5(10) 3_565 3_665 ?
B1 Ca1 B1 145.2(4) 4_466 3_665 ?
O1 Ca1 Si1 23.23(16) 3_565 3_565 ?
O1 Ca1 Si1 94.29(19) . 3_565 ?
O4 Ca1 Si1 98.2(3) 2 3_565 ?
O2 Ca1 Si1 81.8(2) 3_665 3_565 ?
O3 Ca1 Si1 121.14(14) 2_655 3_565 ?
O3 Ca1 Si1 86.59(19) 1_455 3_565 ?
O5 Ca1 Si1 156.5(3) 4_566 3_565 ?
O5 Ca1 Si1 56.3(3) 3_565 3_565 ?
B1 Ca1 Si1 94.9(6) 4_466 3_565 ?
B1 Ca1 Si1 101.5(4) 3_665 3_565 ?
O1 Ca1 Si1 93.0(2) 3_565 . ?
O1 Ca1 Si1 21.98(15) . . ?
O4 Ca1 Si1 125.69(13) 2 . ?
O2 Ca1 Si1 85.6(2) 3_665 . ?
O3 Ca1 Si1 104.8(2) 2_655 . ?
O3 Ca1 Si1 80.8(2) 1_455 . ?
O5 Ca1 Si1 55.1(4) 4_566 . ?
O5 Ca1 Si1 159.1(5) 3_565 . ?
B1 Ca1 Si1 103.3(5) 4_466 . ?
B1 Ca1 Si1 97.0(6) 3_665 . ?
Si1 Ca1 Si1 115.55(7) 3_565 . ?
O1 Si1 O2 117.9(3) . . ?
O1 Si1 O3 116.9(3) . . ?
O2 Si1 O3 105.3(5) . . ?
O1 Si1 O4 106.4(6) . . ?
O2 Si1 O4 103.9(3) . . ?
O3 Si1 O4 105.0(3) . . ?
O1 Si1 Ca1 34.11(12) . 3_565 ?
O2 Si1 Ca1 90.8(3) . 3_565 ?
O3 Si1 Ca1 149.79(17) . 3_565 ?
O4 Si1 Ca1 95.4(3) . 3_565 ?
O1 Si1 Ca1 32.19(13) . . ?
O2 Si1 Ca1 148.20(14) . . ?
O3 Si1 Ca1 90.3(3) . . ?
O4 Si1 Ca1 98.3(4) . . ?
Ca1 Si1 Ca1 64.45(7) 3_565 . ?
O1 Si1 Ca1 95.9(3) . 3_665 ?
O2 Si1 Ca1 36.45(16) . 3_665 ?
O3 Si1 Ca1 93.0(3) . 3_665 ?
O4 Si1 Ca1 140.2(2) . 3_665 ?
Ca1 Si1 Ca1 84.85(6) 3_565 3_665 ?
Ca1 Si1 Ca1 117.02(6) . 3_665 ?
O1 Si1 Ca1 94.1(3) . 1_655 ?
O2 Si1 Ca1 90.9(3) . 1_655 ?
O3 Si1 Ca1 39.48(17) . 1_655 ?
O4 Si1 Ca1 144.5(2) . 1_655 ?
Ca1 Si1 Ca1 116.81(6) 3_565 1_655 ?
Ca1 Si1 Ca1 83.70(6) . 1_655 ?
Ca1 Si1 Ca1 62.41(7) 3_665 1_655 ?
O1 Si1 Ca1 152.07(11) . 2_645 ?
O2 Si1 Ca1 85.6(3) . 2_645 ?
O3 Si1 Ca1 37.00(16) . 2_645 ?
O4 Si1 Ca1 80.0(3) . 2_645 ?
Ca1 Si1 Ca1 173.21(4) 3_565 2_645 ?
Ca1 Si1 Ca1 120.90(5) . 2_645 ?
Ca1 Si1 Ca1 95.56(14) 3_665 2_645 ?
Ca1 Si1 Ca1 69.07(8) 1_655 2_645 ?
O1 Si1 Ca1 89.7(3) . 2_545 ?
O2 Si1 Ca1 136.52(16) . 2_545 ?
O3 Si1 Ca1 88.4(3) . 2_545 ?
O4 Si1 Ca1 33.0(2) . 2_545 ?
Ca1 Si1 Ca1 97.39(15) 3_565 2_545 ?
Ca1 Si1 Ca1 69.93(8) . 2_545 ?
Ca1 Si1 Ca1 172.87(6) 3_665 2_545 ?
Ca1 Si1 Ca1 121.77(5) 1_655 2_545 ?
Ca1 Si1 Ca1 81.42(5) 2_645 2_545 ?
O4 B1 O2 109.8(13) 3_655 . ?
O4 B1 O3 109.0(19) 3_655 4_565 ?
O2 B1 O3 108.4(18) . 4_565 ?
O4 B1 O5 111(2) 3_655 . ?
O2 B1 O5 110(2) . . ?
O3 B1 O5 108.5(11) 4_565 . ?
O4 B1 Ca1 52.0(11) 3_655 4_665 ?
O2 B1 Ca1 119(2) . 4_665 ?
O3 B1 Ca1 57.3(10) 4_565 4_665 ?
O5 B1 Ca1 131.1(5) . 4_665 ?
O4 B1 Ca1 122(2) 3_655 3_665 ?
O2 B1 Ca1 53.1(10) . 3_665 ?
O3 B1 Ca1 55.4(9) 4_565 3_665 ?
O5 B1 Ca1 127.0(6) . 3_665 ?
Ca1 B1 Ca1 85.9(11) 4_665 3_665 ?
Si1 O1 Ca1 122.66(18) . 3_565 ?
Si1 O1 Ca1 125.83(16) . . ?
Ca1 O1 Ca1 107.4(4) 3_565 . ?
B1 O2 Si1 122.4(18) . . ?
B1 O2 Ca1 97.1(11) . 3_665 ?
Si1 O2 Ca1 119.11(15) . 3_665 ?
B1 O3 Si1 122.2(16) 4_566 . ?
B1 O3 Ca1 94.5(8) 4_566 2_645 ?
Si1 O3 Ca1 118.67(16) . 2_645 ?
B1 O3 Ca1 92.4(9) 4_566 1_655 ?
Si1 O3 Ca1 115.12(15) . 1_655 ?
Ca1 O3 Ca1 109.5(4) 2_645 1_655 ?
B1 O4 Si1 127.6(19) 3_655 . ?
B1 O4 Ca1 99.0(13) 3_655 2_545 ?
Si1 O4 Ca1 124.08(19) . 2_545 ?
B1 O5 Ca1 118.1(9) . 4_565 ?
B1 O5 Ca1 121.4(9) . 3_565 ?
Ca1 O5 Ca1 105.8(7) 4_565 3_565 ?
B1 O5 H 146(7) . . ?
Ca1 O5 H 74(7) 4_565 . ?
Ca1 O5 H 80(6) 3_565 . ?

_refine_diff_density_max         0.491
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.137



# start Validation Reply Form
_vrf_PLAT029_shelx               
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.330 Why?  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT051_shelx               
;
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by .      81.71 %     
RESPONSE: ...
;
_vrf_PLAT213_shelx               
;
PROBLEM: Atom Si1             has ADP max/min Ratio .....        7.1 prolat
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT250_shelx               
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....       20.3 Note  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT088_shelx               
;
PROBLEM: Poor Data / Parameter Ratio ....................       6.26 Note  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT911_shelx               
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        173 Report
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1831441'
_audit_update_record             
;
2018-03-21 deposited with the CCDC.
2018-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B Ca H O5 Si'
_chemical_formula_weight         159.99

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0522 0.0431 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0004 0.0004 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.1611 0.1926 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   4.4839(18)
_cell_length_b                   7.2240(10)
_cell_length_c                   9.3484(6)
_cell_angle_alpha                90
_cell_angle_beta                 90.696(18)
_cell_angle_gamma                90
_cell_volume                     302.79(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1403
_cell_measurement_theta_min      1.496
_cell_measurement_theta_max      17.242

_exptl_crystal_description       isosymmetric
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    3.510
_exptl_crystal_F_000             320
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.010
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.005
_exptl_absorpt_coefficient_mu    1.195
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.2984
_diffrn_radiation_type           ?
_diffrn_source                   ?
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            1403
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.496
_diffrn_reflns_theta_max         17.242
_diffrn_reflns_theta_full        10.314
_diffrn_measured_fraction_theta_max 0.293
_diffrn_measured_fraction_theta_full 0.504
_diffrn_reflns_Laue_measured_fraction_max 0.293
_diffrn_reflns_Laue_measured_fraction_full 0.504
_diffrn_reflns_point_group_measured_fraction_max 0.293
_diffrn_reflns_point_group_measured_fraction_full 0.504
_reflns_number_total             726
_reflns_number_gt                634
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1527P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         726
_refine_ls_number_parameters     77
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0547
_refine_ls_wR_factor_ref         0.1594
_refine_ls_wR_factor_gt          0.1475
_refine_ls_goodness_of_fit_ref   0.895
_refine_ls_restrained_S_all      0.894
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.0048(2) 0.61039(6) 0.17001(5) 0.0116(4) Uani 1 1 d . . . . .
Si1 Si 0.4886(3) 0.28047(9) 0.08065(7) 0.0105(5) Uani 1 1 d . . . . .
B1 B 0.5838(12) 0.0827(3) -0.1552(3) 0.0090(14) Uani 1 1 d . . . . .
O1 O 0.2519(8) 0.4230(3) 0.0300(2) 0.0121(11) Uani 1 1 d . . . . .
O2 O 0.7081(8) 0.1918(3) -0.03705(19) 0.0109(10) Uani 1 1 d . . . . .
O3 O 0.7032(8) 0.3413(3) 0.21330(19) 0.0108(10) Uani 1 1 d . . . . .
O4 O 0.3006(9) 0.1027(2) 0.1404(2) 0.0126(10) Uani 1 1 d . . . . .
O5 O 0.2590(8) 0.0900(3) -0.1609(2) 0.0112(11) Uani 1 1 d D . . . .
H H 0.208(14) 0.043(4) -0.075(3) 0.002(9) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O1 2.193(3) . ?
Ca1 O1 2.197(2) 3_565 ?
Ca1 O4 2.254(4) 2 ?
Ca1 O2 2.299(3) 3_665 ?
Ca1 O3 2.378(2) 2_655 ?
Ca1 O3 2.405(3) 1_455 ?
Ca1 O5 2.419(2) 4_566 ?
Ca1 O5 2.467(3) 3_565 ?
Ca1 B1 2.873(5) 4_466 ?
Ca1 B1 2.888(4) 3_665 ?
Ca1 Si1 3.2986(13) 3_565 ?
Ca1 Si1 3.3360(15) . ?
Si1 O1 1.548(3) . ?
Si1 O2 1.617(4) . ?
Si1 O3 1.621(2) . ?
Si1 O4 1.638(3) . ?
Si1 Ca1 3.2986(13) 3_565 ?
Si1 Ca1 3.3768(17) 3_665 ?
Si1 Ca1 3.4187(14) 1_655 ?
Si1 Ca1 3.4586(16) 2_545 ?
Si1 Ca1 3.4604(13) 2_645 ?
B1 O4 1.442(4) 3_655 ?
B1 O3 1.454(5) 4_565 ?
B1 O5 1.458(7) . ?
B1 O2 1.462(3) . ?
B1 Ca1 2.873(5) 4_665 ?
B1 Ca1 2.888(4) 3_665 ?
O1 Ca1 2.197(2) 3_565 ?
O2 Ca1 2.299(3) 3_665 ?
O3 B1 1.454(5) 4_566 ?
O3 Ca1 2.378(2) 2_645 ?
O3 Ca1 2.405(3) 1_655 ?
O4 B1 1.442(4) 3_655 ?
O4 Ca1 2.254(4) 2_545 ?
O5 Ca1 2.419(2) 4_565 ?
O5 Ca1 2.467(3) 3_565 ?
O5 H 0.90(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ca1 O1 71.80(14) . 3_565 ?
O1 Ca1 O4 140.39(9) . 2 ?
O1 Ca1 O4 110.46(13) 3_565 2 ?
O1 Ca1 O2 76.75(11) . 3_665 ?
O1 Ca1 O2 84.20(10) 3_565 3_665 ?
O4 Ca1 O2 142.22(8) 2 3_665 ?
O1 Ca1 O3 115.32(12) . 2_655 ?
O1 Ca1 O3 138.36(8) 3_565 2_655 ?
O4 Ca1 O3 89.60(9) 2 2_655 ?
O2 Ca1 O3 60.19(7) 3_665 2_655 ?
O1 Ca1 O3 83.72(11) . 1_455 ?
O1 Ca1 O3 76.40(9) 3_565 1_455 ?
O4 Ca1 O3 59.96(8) 2 1_455 ?
O2 Ca1 O3 155.96(7) 3_665 1_455 ?
O3 Ca1 O3 142.90(4) 2_655 1_455 ?
O1 Ca1 O5 77.46(8) . 4_566 ?
O1 Ca1 O5 136.76(7) 3_565 4_566 ?
O4 Ca1 O5 75.95(10) 2 4_566 ?
O2 Ca1 O5 117.57(12) 3_665 4_566 ?
O3 Ca1 O5 82.39(7) 2_655 4_566 ?
O3 Ca1 O5 70.59(9) 1_455 4_566 ?
O1 Ca1 O5 140.03(8) . 3_565 ?
O1 Ca1 O5 79.67(7) 3_565 3_565 ?
O4 Ca1 O5 75.71(9) 2 3_565 ?
O2 Ca1 O5 72.99(11) 3_665 3_565 ?
O3 Ca1 O5 70.22(9) 2_655 3_565 ?
O3 Ca1 O5 116.39(12) 1_455 3_565 ?
O5 Ca1 O5 140.32(5) 4_566 3_565 ?
O1 Ca1 B1 112.32(10) . 4_466 ?
O1 Ca1 B1 95.15(12) 3_565 4_466 ?
O4 Ca1 B1 29.66(8) 2 4_466 ?
O2 Ca1 B1 170.27(11) 3_665 4_466 ?
O3 Ca1 B1 116.22(9) 2_655 4_466 ?
O3 Ca1 B1 30.36(8) 1_455 4_466 ?
O5 Ca1 B1 69.23(12) 4_566 4_466 ?
O5 Ca1 B1 97.33(12) 3_565 4_466 ?
O1 Ca1 B1 96.76(13) . 3_665 ?
O1 Ca1 B1 111.82(9) 3_565 3_665 ?
O4 Ca1 B1 116.82(9) 2 3_665 ?
O2 Ca1 B1 30.08(7) 3_665 3_665 ?
O3 Ca1 B1 30.11(9) 2_655 3_665 ?
O3 Ca1 B1 171.54(8) 1_455 3_665 ?
O5 Ca1 B1 101.22(10) 4_566 3_665 ?
O5 Ca1 B1 68.37(13) 3_565 3_665 ?
B1 Ca1 B1 145.52(7) 4_466 3_665 ?
O1 Ca1 Si1 93.61(6) . 3_565 ?
O1 Ca1 Si1 23.32(7) 3_565 3_565 ?
O4 Ca1 Si1 98.97(9) 2 3_565 ?
O2 Ca1 Si1 80.94(7) 3_665 3_565 ?
O3 Ca1 Si1 121.27(5) 2_655 3_565 ?
O3 Ca1 Si1 86.51(6) 1_455 3_565 ?
O5 Ca1 Si1 156.07(7) 4_566 3_565 ?
O5 Ca1 Si1 56.54(5) 3_565 3_565 ?
B1 Ca1 Si1 94.62(8) 4_466 3_565 ?
B1 Ca1 Si1 101.87(6) 3_665 3_565 ?
O1 Ca1 Si1 22.27(5) . . ?
O1 Ca1 Si1 92.53(8) 3_565 . ?
O4 Ca1 Si1 125.63(6) 2 . ?
O2 Ca1 Si1 86.48(9) 3_665 . ?
O3 Ca1 Si1 105.07(9) 2_655 . ?
O3 Ca1 Si1 80.41(8) 1_455 . ?
O5 Ca1 Si1 55.48(7) 4_566 . ?
O5 Ca1 Si1 158.59(8) 3_565 . ?
B1 Ca1 Si1 103.25(8) 4_466 . ?
B1 Ca1 Si1 96.82(10) 3_665 . ?
Si1 Ca1 Si1 115.18(3) 3_565 . ?
O1 Si1 O2 118.41(13) . . ?
O1 Si1 O3 116.86(12) . . ?
O2 Si1 O3 105.50(17) . . ?
O1 Si1 O4 105.77(18) . . ?
O2 Si1 O4 103.96(14) . . ?
O3 Si1 O4 104.78(11) . . ?
O1 Si1 Ca1 34.17(7) . 3_565 ?
O2 Si1 Ca1 91.13(8) . 3_565 ?
O3 Si1 Ca1 149.92(8) . 3_565 ?
O4 Si1 Ca1 94.94(10) . 3_565 ?
O1 Si1 Ca1 32.47(9) . . ?
O2 Si1 Ca1 148.90(7) . . ?
O3 Si1 Ca1 89.80(11) . . ?
O4 Si1 Ca1 97.81(13) . . ?
Ca1 Si1 Ca1 64.82(3) 3_565 . ?
O1 Si1 Ca1 95.56(13) . 3_665 ?
O2 Si1 Ca1 36.90(8) . 3_665 ?
O3 Si1 Ca1 93.98(13) . 3_665 ?
O4 Si1 Ca1 140.62(11) . 3_665 ?
Ca1 Si1 Ca1 84.39(3) 3_565 3_665 ?
Ca1 Si1 Ca1 116.87(3) . 3_665 ?
O1 Si1 Ca1 94.06(11) . 1_655 ?
O2 Si1 Ca1 91.52(11) . 1_655 ?
O3 Si1 Ca1 39.66(9) . 1_655 ?
O4 Si1 Ca1 144.38(8) . 1_655 ?
Ca1 Si1 Ca1 116.95(3) 3_565 1_655 ?
Ca1 Si1 Ca1 83.17(3) . 1_655 ?
Ca1 Si1 Ca1 63.11(3) 3_665 1_655 ?
O1 Si1 Ca1 90.03(14) . 2_545 ?
O2 Si1 Ca1 135.83(8) . 2_545 ?
O3 Si1 Ca1 87.68(12) . 2_545 ?
O4 Si1 Ca1 32.41(10) . 2_545 ?
Ca1 Si1 Ca1 97.74(5) 3_565 2_545 ?
Ca1 Si1 Ca1 70.23(3) . 2_545 ?
Ca1 Si1 Ca1 172.67(3) 3_665 2_545 ?
Ca1 Si1 Ca1 121.31(3) 1_655 2_545 ?
O1 Si1 Ca1 152.11(8) . 2_645 ?
O2 Si1 Ca1 85.28(9) . 2_645 ?
O3 Si1 Ca1 37.09(8) . 2_645 ?
O4 Si1 Ca1 80.11(10) . 2_645 ?
Ca1 Si1 Ca1 172.98(2) 3_565 2_645 ?
Ca1 Si1 Ca1 120.57(3) . 2_645 ?
Ca1 Si1 Ca1 96.24(5) 3_665 2_645 ?
Ca1 Si1 Ca1 69.27(3) 1_655 2_645 ?
Ca1 Si1 Ca1 80.79(3) 2_545 2_645 ?
O4 B1 O3 107.2(3) 3_655 4_565 ?
O4 B1 O5 113.3(3) 3_655 . ?
O3 B1 O5 109.5(2) 4_565 . ?
O4 B1 O2 107.1(2) 3_655 . ?
O3 B1 O2 107.1(3) 4_565 . ?
O5 B1 O2 112.3(3) . . ?
O4 B1 Ca1 50.6(2) 3_655 4_665 ?
O3 B1 Ca1 56.71(18) 4_565 4_665 ?
O5 B1 Ca1 131.29(16) . 4_665 ?
O2 B1 Ca1 116.4(3) . 4_665 ?
O4 B1 Ca1 119.2(3) 3_655 3_665 ?
O3 B1 Ca1 55.11(16) 4_565 3_665 ?
O5 B1 Ca1 127.50(16) . 3_665 ?
O2 B1 Ca1 52.02(18) . 3_665 ?
Ca1 B1 Ca1 85.47(15) 4_665 3_665 ?
Si1 O1 Ca1 125.26(11) . . ?
Si1 O1 Ca1 122.51(12) . 3_565 ?
Ca1 O1 Ca1 108.20(14) . 3_565 ?
B1 O2 Si1 119.9(3) . . ?
B1 O2 Ca1 97.9(2) . 3_665 ?
Si1 O2 Ca1 118.10(10) . 3_665 ?
B1 O3 Si1 121.8(3) 4_566 . ?
B1 O3 Ca1 94.77(15) 4_566 2_645 ?
Si1 O3 Ca1 118.62(10) . 2_645 ?
B1 O3 Ca1 92.92(17) 4_566 1_655 ?
Si1 O3 Ca1 114.85(10) . 1_655 ?
Ca1 O3 Ca1 109.68(13) 2_645 1_655 ?
B1 O4 Si1 125.1(4) 3_655 . ?
B1 O4 Ca1 99.7(2) 3_655 2_545 ?
Si1 O4 Ca1 124.67(12) . 2_545 ?
B1 O5 Ca1 117.70(19) . 4_565 ?
B1 O5 Ca1 120.76(16) . 3_565 ?
Ca1 O5 Ca1 106.29(10) 4_565 3_565 ?
B1 O5 H 102(4) . . ?
Ca1 O5 H 104(3) 4_565 . ?
Ca1 O5 H 104(3) 3_565 . ?

_refine_diff_density_max         1.062
_refine_diff_density_min         -1.262
_refine_diff_density_rms         0.180



# start Validation Reply Form
_vrf_PLAT029_shelx               
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.504 Why?  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT051_shelx               
;
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by .      80.46 %     
RESPONSE: ...
;
_vrf_PLAT250_shelx               
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        4.3 Note  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT911_shelx               
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        274 Report
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1831444'
_audit_update_record             
;
2018-03-21 deposited with the CCDC.
2018-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B Ca H O5 Si'
_chemical_formula_weight         159.99

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0522 0.0431 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0004 0.0004 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.1611 0.1926 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   4.479(7)
_cell_length_b                   6.7168(6)
_cell_length_c                   9.2421(7)
_cell_angle_alpha                90
_cell_angle_beta                 90.63(3)
_cell_angle_gamma                90
_cell_volume                     278.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1051
_cell_measurement_theta_min      1.527
_cell_measurement_theta_max      17.450

_exptl_crystal_description       isosymmetric
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    3.822
_exptl_crystal_F_000             320
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.010
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.005
_exptl_absorpt_coefficient_mu    1.301
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.2896
_diffrn_radiation_type           ?
_diffrn_source                   ?
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            1051
_diffrn_reflns_av_unetI/netI     0.0774
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_h_max       2
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.527
_diffrn_reflns_theta_max         17.450
_diffrn_reflns_theta_full        10.007
_diffrn_measured_fraction_theta_max 0.192
_diffrn_measured_fraction_theta_full 0.336
_diffrn_reflns_Laue_measured_fraction_max 0.192
_diffrn_reflns_Laue_measured_fraction_full 0.336
_diffrn_reflns_point_group_measured_fraction_max 0.192
_diffrn_reflns_point_group_measured_fraction_full 0.336
_reflns_number_total             498
_reflns_number_gt                376
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1423P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         498
_refine_ls_number_parameters     71
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0594
_refine_ls_wR_factor_ref         0.1693
_refine_ls_wR_factor_gt          0.1485
_refine_ls_goodness_of_fit_ref   0.834
_refine_ls_restrained_S_all      0.833
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.0002(6) 0.63005(10) 0.18073(8) 0.0212(19) Uani 1 1 d . . . . .
Si1 Si 0.5312(9) 0.32208(16) 0.06636(11) 0.021(2) Uani 1 1 d . . . . .
B1 B 0.592(5) 0.0580(6) -0.1520(6) 0.0080(7) Uiso 1 1 d . . . . .
O1 O 0.260(3) 0.4607(5) 0.0160(3) 0.020(6) Uani 1 1 d . . . . .
O2 O 0.725(3) 0.1775(4) -0.0381(3) 0.025(6) Uani 1 1 d . . . . .
O3 O 0.708(3) 0.3631(4) 0.2158(3) 0.027(6) Uani 1 1 d . . . . .
O4 O 0.313(2) 0.1407(4) 0.1316(3) 0.028(6) Uani 1 1 d . . . . .
O5 O 0.266(3) 0.0772(4) -0.1594(3) 0.027(7) Uani 1 1 d D . . . .
H H 0.149(19) 0.027(9) -0.090(7) 0.010 Uiso 1 1 d D U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O2 2.228(8) 3_665 ?
Ca1 O1 2.233(7) 3_565 ?
Ca1 O1 2.237(8) . ?
Ca1 O4 2.244(8) 2 ?
Ca1 O3 2.246(7) 1_455 ?
Ca1 O3 2.247(7) 2_655 ?
Ca1 O5 2.306(7) 3_565 ?
Ca1 O5 2.345(6) 4_566 ?
Ca1 B1 2.717(15) 4_466 ?
Ca1 B1 2.793(15) 3_665 ?
Ca1 Si1 3.124(4) 1_455 ?
Ca1 Si1 3.135(4) 3_665 ?
Si1 O1 1.597(11) . ?
Si1 O3 1.608(6) . ?
Si1 O2 1.626(7) . ?
Si1 O4 1.678(7) . ?
Si1 O1 1.897(7) 3_665 ?
Si1 Si1 2.700(2) 3_665 ?
Si1 Ca1 3.124(4) 1_655 ?
Si1 Ca1 3.135(4) 3_665 ?
Si1 Ca1 3.296(5) 3_565 ?
Si1 Ca1 3.380(4) 2_645 ?
Si1 Ca1 3.594(4) 2_545 ?
B1 O4 1.412(8) 3_655 ?
B1 O3 1.433(12) 4_565 ?
B1 O2 1.445(10) . ?
B1 O5 1.47(2) . ?
B1 Ca1 2.717(15) 4_665 ?
B1 Ca1 2.793(15) 3_665 ?
O1 Si1 1.897(7) 3_665 ?
O1 Ca1 2.233(7) 3_565 ?
O2 Ca1 2.228(8) 3_665 ?
O3 B1 1.433(12) 4_566 ?
O3 Ca1 2.246(7) 1_655 ?
O3 Ca1 2.247(7) 2_645 ?
O4 B1 1.412(8) 3_655 ?
O4 Ca1 2.244(8) 2_545 ?
O5 Ca1 2.306(7) 3_565 ?
O5 Ca1 2.345(6) 4_565 ?
O5 H 0.90(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ca1 O1 87.9(3) 3_665 3_565 ?
O2 Ca1 O1 66.3(2) 3_665 . ?
O1 Ca1 O1 65.0(5) 3_565 . ?
O2 Ca1 O4 142.50(14) 3_665 2 ?
O1 Ca1 O4 108.2(4) 3_565 2 ?
O1 Ca1 O4 151.22(17) . 2 ?
O2 Ca1 O3 151.16(12) 3_665 1_455 ?
O1 Ca1 O3 66.4(2) 3_565 1_455 ?
O1 Ca1 O3 90.0(3) . 1_455 ?
O4 Ca1 O3 62.8(2) 2 1_455 ?
O2 Ca1 O3 61.59(18) 3_665 2_655 ?
O1 Ca1 O3 146.36(15) 3_565 2_655 ?
O1 Ca1 O3 109.9(4) . 2_655 ?
O4 Ca1 O3 90.8(3) 2 2_655 ?
O3 Ca1 O3 146.35(12) 1_455 2_655 ?
O2 Ca1 O5 75.1(3) 3_665 3_565 ?
O1 Ca1 O5 84.2(2) 3_565 3_565 ?
O1 Ca1 O5 130.34(16) . 3_565 ?
O4 Ca1 O5 73.3(2) 2 3_565 ?
O3 Ca1 O5 113.0(4) 1_455 3_565 ?
O3 Ca1 O5 74.9(3) 2_655 3_565 ?
O2 Ca1 O5 115.9(4) 3_665 4_566 ?
O1 Ca1 O5 127.40(16) 3_565 4_566 ?
O1 Ca1 O5 82.1(2) . 4_566 ?
O4 Ca1 O5 81.3(3) 2 4_566 ?
O3 Ca1 O5 74.2(3) 1_455 4_566 ?
O3 Ca1 O5 81.8(2) 2_655 4_566 ?
O5 Ca1 O5 144.89(12) 3_565 4_566 ?
O2 Ca1 B1 170.4(4) 3_665 4_466 ?
O1 Ca1 B1 89.4(3) 3_565 4_466 ?
O1 Ca1 B1 120.6(2) . 4_466 ?
O4 Ca1 B1 31.26(16) 2 4_466 ?
O3 Ca1 B1 31.80(17) 1_455 4_466 ?
O3 Ca1 B1 118.3(2) 2_655 4_466 ?
O5 Ca1 B1 95.5(4) 3_565 4_466 ?
O5 Ca1 B1 72.8(4) 4_566 4_466 ?
O2 Ca1 B1 30.92(16) 3_665 3_665 ?
O1 Ca1 B1 117.6(2) 3_565 3_665 ?
O1 Ca1 B1 88.4(3) . 3_665 ?
O4 Ca1 B1 117.7(2) 2 3_665 ?
O3 Ca1 B1 174.4(4) 1_455 3_665 ?
O3 Ca1 B1 30.67(16) 2_655 3_665 ?
O5 Ca1 B1 71.9(4) 3_565 3_665 ?
O5 Ca1 B1 100.2(3) 4_566 3_665 ?
B1 Ca1 B1 147.86(19) 4_466 3_665 ?
O2 Ca1 Si1 123.94(14) 3_665 1_455 ?
O1 Ca1 Si1 36.98(17) 3_565 1_455 ?
O1 Ca1 Si1 77.6(3) . 1_455 ?
O4 Ca1 Si1 81.9(2) 2 1_455 ?
O3 Ca1 Si1 29.46(11) 1_455 1_455 ?
O3 Ca1 Si1 172.5(3) 2_655 1_455 ?
O5 Ca1 Si1 101.0(3) 3_565 1_455 ?
O5 Ca1 Si1 98.89(19) 4_566 1_455 ?
B1 Ca1 Si1 55.33(17) 4_466 1_455 ?
B1 Ca1 Si1 154.43(12) 3_665 1_455 ?
O2 Ca1 Si1 29.59(14) 3_665 3_665 ?
O1 Ca1 Si1 77.4(3) 3_565 3_665 ?
O1 Ca1 Si1 36.79(16) . 3_665 ?
O4 Ca1 Si1 171.50(13) 2 3_665 ?
O3 Ca1 Si1 125.67(16) 1_455 3_665 ?
O3 Ca1 Si1 81.2(2) 2_655 3_665 ?
O5 Ca1 Si1 101.5(2) 3_565 3_665 ?
O5 Ca1 Si1 100.4(3) 4_566 3_665 ?
B1 Ca1 Si1 157.18(14) 4_466 3_665 ?
B1 Ca1 Si1 53.9(2) 3_665 3_665 ?
Si1 Ca1 Si1 105.93(10) 1_455 3_665 ?
O1 Si1 O3 121.1(3) . . ?
O1 Si1 O2 125.7(3) . . ?
O3 Si1 O2 110.6(5) . . ?
O1 Si1 O4 94.8(5) . . ?
O3 Si1 O4 95.7(3) . . ?
O2 Si1 O4 95.5(3) . . ?
O1 Si1 O1 79.2(6) . 3_665 ?
O3 Si1 O1 88.4(3) . 3_665 ?
O2 Si1 O1 87.3(4) . 3_665 ?
O4 Si1 O1 173.9(5) . 3_665 ?
O1 Si1 Si1 43.7(3) . 3_665 ?
O3 Si1 Si1 106.62(15) . 3_665 ?
O2 Si1 Si1 108.20(17) . 3_665 ?
O4 Si1 Si1 138.4(4) . 3_665 ?
O1 Si1 Si1 35.5(3) 3_665 3_665 ?
O1 Si1 Ca1 102.7(3) . 1_655 ?
O3 Si1 Ca1 43.4(2) . 1_655 ?
O2 Si1 Ca1 103.6(4) . 1_655 ?
O4 Si1 Ca1 138.69(16) . 1_655 ?
O1 Si1 Ca1 45.05(18) 3_665 1_655 ?
Si1 Si1 Ca1 68.49(12) 3_665 1_655 ?
O1 Si1 Ca1 104.0(3) . 3_665 ?
O3 Si1 Ca1 106.3(4) . 3_665 ?
O2 Si1 Ca1 42.6(2) . 3_665 ?
O4 Si1 Ca1 137.17(19) . 3_665 ?
O1 Si1 Ca1 44.9(2) 3_665 3_665 ?
Si1 Si1 Ca1 69.21(12) 3_665 3_665 ?
Ca1 Si1 Ca1 74.07(10) 1_655 3_665 ?
O1 Si1 Ca1 36.80(13) . 3_565 ?
O3 Si1 Ca1 157.4(3) . 3_565 ?
O2 Si1 Ca1 91.8(3) . 3_565 ?
O4 Si1 Ca1 84.3(3) . 3_565 ?
O1 Si1 Ca1 90.2(3) 3_665 3_565 ?
Si1 Si1 Ca1 61.86(12) 3_665 3_565 ?
Ca1 Si1 Ca1 130.36(6) 1_655 3_565 ?
Ca1 Si1 Ca1 88.25(9) 3_665 3_565 ?
O1 Si1 Ca1 35.60(16) . . ?
O3 Si1 Ca1 88.1(3) . . ?
O2 Si1 Ca1 161.0(3) . . ?
O4 Si1 Ca1 85.2(3) . . ?
O1 Si1 Ca1 90.4(3) 3_665 . ?
Si1 Si1 Ca1 61.57(12) 3_665 . ?
Ca1 Si1 Ca1 87.78(9) 1_655 . ?
Ca1 Si1 Ca1 130.78(6) 3_665 . ?
Ca1 Si1 Ca1 69.31(10) 3_565 . ?
O1 Si1 Ca1 152.78(16) . 2_645 ?
O3 Si1 Ca1 34.47(19) . 2_645 ?
O2 Si1 Ca1 81.5(3) . 2_645 ?
O4 Si1 Ca1 80.4(3) . 2_645 ?
O1 Si1 Ca1 105.4(3) 3_665 2_645 ?
Si1 Si1 Ca1 135.44(18) 3_665 2_645 ?
Ca1 Si1 Ca1 66.96(8) 1_655 2_645 ?
Ca1 Si1 Ca1 97.32(16) 3_665 2_645 ?
Ca1 Si1 Ca1 162.66(7) 3_565 2_645 ?
Ca1 Si1 Ca1 117.22(7) . 2_645 ?
O1 Si1 Ca1 83.8(3) . 2_545 ?
O3 Si1 Ca1 80.0(3) . 2_545 ?
O2 Si1 Ca1 122.2(2) . 2_545 ?
O4 Si1 Ca1 27.52(17) . 2_545 ?
O1 Si1 Ca1 150.5(2) 3_665 2_545 ?
Si1 Si1 Ca1 123.2(2) 3_665 2_545 ?
Ca1 Si1 Ca1 117.72(7) 1_655 2_545 ?
Ca1 Si1 Ca1 164.60(4) 3_665 2_545 ?
Ca1 Si1 Ca1 90.42(15) 3_565 2_545 ?
Ca1 Si1 Ca1 62.38(8) . 2_545 ?
Ca1 Si1 Ca1 79.86(9) 2_645 2_545 ?
O4 B1 O3 110.6(10) 3_655 4_565 ?
O4 B1 O2 107.9(8) 3_655 . ?
O3 B1 O2 105.5(9) 4_565 . ?
O4 B1 O5 112.7(11) 3_655 . ?
O3 B1 O5 107.2(8) 4_565 . ?
O2 B1 O5 112.6(9) . . ?
O4 B1 Ca1 55.5(6) 3_655 4_665 ?
O3 B1 Ca1 55.7(6) 4_565 4_665 ?
O2 B1 Ca1 113.6(11) . 4_665 ?
O5 B1 Ca1 133.6(4) . 4_665 ?
O4 B1 Ca1 121.8(12) 3_655 3_665 ?
O3 B1 Ca1 53.1(5) 4_565 3_665 ?
O2 B1 Ca1 52.4(5) . 3_665 ?
O5 B1 Ca1 125.5(3) . 3_665 ?
Ca1 B1 Ca1 81.4(5) 4_665 3_665 ?
Si1 O1 Si1 100.8(6) . 3_665 ?
Si1 O1 Ca1 117.8(2) . 3_565 ?
Si1 O1 Ca1 97.97(15) 3_665 3_565 ?
Si1 O1 Ca1 119.85(19) . . ?
Si1 O1 Ca1 98.30(16) 3_665 . ?
Ca1 O1 Ca1 115.0(5) 3_565 . ?
B1 O2 Si1 123.2(11) . . ?
B1 O2 Ca1 96.7(5) . 3_665 ?
Si1 O2 Ca1 107.84(18) . 3_665 ?
B1 O3 Si1 128.1(11) 4_566 . ?
B1 O3 Ca1 92.5(5) 4_566 1_655 ?
Si1 O3 Ca1 107.2(2) . 1_655 ?
B1 O3 Ca1 96.2(5) 4_566 2_645 ?
Si1 O3 Ca1 121.64(19) . 2_645 ?
Ca1 O3 Ca1 106.3(5) 1_655 2_645 ?
B1 O4 Si1 124.0(11) 3_655 . ?
B1 O4 Ca1 93.2(6) 3_655 2_545 ?
Si1 O4 Ca1 132.27(19) . 2_545 ?
B1 O5 Ca1 126.3(4) . 3_565 ?
B1 O5 Ca1 118.4(3) . 4_565 ?
Ca1 O5 Ca1 101.2(4) 3_565 4_565 ?
B1 O5 H 121(6) . . ?
Ca1 O5 H 94(5) 3_565 . ?
Ca1 O5 H 86(5) 4_565 . ?

_refine_diff_density_max         0.715
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.187



# start Validation Reply Form
_vrf_PLAT029_shelx               
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.336 Why?  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT051_shelx               
;
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by .      81.69 %     
RESPONSE: ...
;
_vrf_PLAT213_shelx               
;
PROBLEM: Atom O2              has ADP max/min Ratio .....        5.1 prolat
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT250_shelx               
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....       12.4 Note  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT088_shelx               
;
PROBLEM: Poor Data / Parameter Ratio ....................       7.01 Note  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT911_shelx               
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        158 Report
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 1831438'
_audit_update_record             
;
2018-03-21 deposited with the CCDC.
2018-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B Ca H O5 Si'
_chemical_formula_weight         159.99

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0522 0.0431 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0004 0.0004 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.1611 0.1926 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   4.6378(17)
_cell_length_b                   7.4034(4)
_cell_length_c                   9.4840(6)
_cell_angle_alpha                90
_cell_angle_beta                 90.729(17)
_cell_angle_gamma                90
_cell_volume                     325.61(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1733
_cell_measurement_theta_min      1.465
_cell_measurement_theta_max      17.349

_exptl_crystal_description       isosymmetric
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    3.264
_exptl_crystal_F_000             320
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.010
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.005
_exptl_absorpt_coefficient_mu    1.111
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.2984
_diffrn_radiation_type           ?
_diffrn_source                   ?
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            1733
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.465
_diffrn_reflns_theta_max         17.349
_diffrn_reflns_theta_full        10.314
_diffrn_measured_fraction_theta_max 0.325
_diffrn_measured_fraction_theta_full 0.552
_diffrn_reflns_Laue_measured_fraction_max 0.325
_diffrn_reflns_Laue_measured_fraction_full 0.552
_diffrn_reflns_point_group_measured_fraction_max 0.325
_diffrn_reflns_point_group_measured_fraction_full 0.552
_reflns_number_total             884
_reflns_number_gt                790
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1541P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.7(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         884
_refine_ls_number_parameters     78
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0480
_refine_ls_wR_factor_ref         0.2087
_refine_ls_wR_factor_gt          0.1709
_refine_ls_goodness_of_fit_ref   1.208
_refine_ls_restrained_S_all      1.207
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.0056(2) 0.60809(6) 0.16715(6) 0.0106(4) Uani 1 1 d . . . . .
Si1 Si 0.4796(3) 0.27333(9) 0.08298(7) 0.0086(5) Uani 1 1 d . . . . .
B1 B 0.5757(11) 0.0862(3) -0.1563(3) 0.0077(11) Uani 1 1 d . . . . .
O1 O 0.2489(7) 0.4135(3) 0.0335(2) 0.0106(10) Uani 1 1 d . . . . .
O2 O 0.6924(8) 0.1960(3) -0.0394(2) 0.0111(9) Uani 1 1 d . . . . .
O3 O 0.6949(8) 0.3374(3) 0.2120(2) 0.0115(9) Uani 1 1 d . . . . .
O4 O 0.3074(9) 0.0952(2) 0.1431(3) 0.0119(9) Uani 1 1 d . . . . .
O5 O 0.2596(8) 0.0893(3) -0.1626(2) 0.0114(10) Uani 1 1 d D . . . .
H H 0.22(2) 0.042(8) -0.079(4) 0.04(2) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O1 2.232(2) 3_565 ?
Ca1 O1 2.234(3) . ?
Ca1 O4 2.328(4) 2 ?
Ca1 O2 2.361(3) 3_665 ?
Ca1 O5 2.466(2) 4_566 ?
Ca1 O3 2.467(2) 2_655 ?
Ca1 O3 2.508(3) 1_455 ?
Ca1 O5 2.556(2) 3_565 ?
Ca1 B1 2.985(4) 3_665 ?
Ca1 B1 2.989(5) 4_466 ?
Ca1 Si1 3.3653(12) 3_565 ?
Ca1 Si1 3.4140(14) . ?
Si1 O1 1.559(3) . ?
Si1 O2 1.636(4) . ?
Si1 O3 1.640(2) . ?
Si1 O4 1.647(3) . ?
Si1 Ca1 3.3654(12) 3_565 ?
Si1 Ca1 3.4990(17) 3_665 ?
Si1 Ca1 3.5088(16) 2_545 ?
Si1 Ca1 3.5594(13) 2_645 ?
Si1 Ca1 3.5613(14) 1_655 ?
B1 O4 1.453(4) 3_655 ?
B1 O5 1.467(6) . ?
B1 O2 1.472(3) . ?
B1 O3 1.484(4) 4_565 ?
B1 Ca1 2.985(4) 3_665 ?
B1 Ca1 2.989(5) 4_665 ?
O1 Ca1 2.232(2) 3_565 ?
O2 Ca1 2.362(3) 3_665 ?
O3 B1 1.484(4) 4_566 ?
O3 Ca1 2.467(2) 2_645 ?
O3 Ca1 2.508(3) 1_655 ?
O4 B1 1.453(4) 3_655 ?
O4 Ca1 2.328(4) 2_545 ?
O5 Ca1 2.466(2) 4_565 ?
O5 Ca1 2.556(2) 3_565 ?
O5 H 0.88(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ca1 O1 74.67(12) 3_565 . ?
O1 Ca1 O4 109.13(12) 3_565 2 ?
O1 Ca1 O4 137.44(8) . 2 ?
O1 Ca1 O2 85.26(10) 3_565 3_665 ?
O1 Ca1 O2 78.32(11) . 3_665 ?
O4 Ca1 O2 143.26(7) 2 3_665 ?
O1 Ca1 O5 139.35(7) 3_565 4_566 ?
O1 Ca1 O5 75.48(8) . 4_566 ?
O4 Ca1 O5 76.52(10) 2 4_566 ?
O2 Ca1 O5 114.74(12) 3_665 4_566 ?
O1 Ca1 O3 137.22(7) 3_565 2_655 ?
O1 Ca1 O3 114.96(12) . 2_655 ?
O4 Ca1 O3 91.26(9) 2 2_655 ?
O2 Ca1 O3 58.77(7) 3_665 2_655 ?
O5 Ca1 O3 80.92(7) 4_566 2_655 ?
O1 Ca1 O3 77.78(8) 3_565 1_455 ?
O1 Ca1 O3 82.91(10) . 1_455 ?
O4 Ca1 O3 58.06(8) 2 1_455 ?
O2 Ca1 O3 157.46(7) 3_665 1_455 ?
O5 Ca1 O3 71.71(9) 4_566 1_455 ?
O3 Ca1 O3 142.43(4) 2_655 1_455 ?
O1 Ca1 O5 78.41(8) 3_565 3_565 ?
O1 Ca1 O5 143.30(8) . 3_565 ?
O4 Ca1 O5 75.19(9) 2 3_565 ?
O2 Ca1 O5 75.01(11) 3_665 3_565 ?
O5 Ca1 O5 139.13(5) 4_566 3_565 ?
O3 Ca1 O5 70.89(9) 2_655 3_565 ?
O3 Ca1 O5 115.20(12) 1_455 3_565 ?
O1 Ca1 B1 111.24(9) 3_565 3_665 ?
O1 Ca1 B1 97.80(12) . 3_665 ?
O4 Ca1 B1 118.03(9) 2 3_665 ?
O2 Ca1 B1 29.10(7) 3_665 3_665 ?
O5 Ca1 B1 99.58(10) 4_566 3_665 ?
O3 Ca1 B1 29.70(8) 2_655 3_665 ?
O3 Ca1 B1 170.86(7) 1_455 3_665 ?
O5 Ca1 B1 69.38(11) 3_565 3_665 ?
O1 Ca1 B1 95.37(11) 3_565 4_466 ?
O1 Ca1 B1 110.67(9) . 4_466 ?
O4 Ca1 B1 28.41(7) 2 4_466 ?
O2 Ca1 B1 170.85(10) 3_665 4_466 ?
O5 Ca1 B1 70.39(11) 4_566 4_466 ?
O3 Ca1 B1 116.53(9) 2_655 4_466 ?
O3 Ca1 B1 29.72(8) 1_455 4_466 ?
O5 Ca1 B1 96.15(11) 3_565 4_466 ?
B1 Ca1 B1 145.40(7) 3_665 4_466 ?
O1 Ca1 Si1 22.51(7) 3_565 3_565 ?
O1 Ca1 Si1 96.09(6) . 3_565 ?
O4 Ca1 Si1 97.91(8) 2 3_565 ?
O2 Ca1 Si1 82.74(7) 3_665 3_565 ?
O5 Ca1 Si1 157.77(6) 4_566 3_565 ?
O3 Ca1 Si1 121.03(5) 2_655 3_565 ?
O3 Ca1 Si1 86.99(6) 1_455 3_565 ?
O5 Ca1 Si1 56.08(5) 3_565 3_565 ?
B1 Ca1 Si1 101.96(6) 3_665 3_565 ?
B1 Ca1 Si1 94.34(8) 4_466 3_565 ?
O1 Ca1 Si1 94.81(8) 3_565 . ?
O1 Ca1 Si1 21.25(5) . . ?
O4 Ca1 Si1 124.10(6) 2 . ?
O2 Ca1 Si1 86.45(8) 3_665 . ?
O5 Ca1 Si1 54.51(7) 4_566 . ?
O3 Ca1 Si1 104.35(8) 2_655 . ?
O3 Ca1 Si1 80.37(8) 1_455 . ?
O5 Ca1 Si1 160.64(8) 3_565 . ?
B1 Ca1 Si1 96.97(9) 3_665 . ?
B1 Ca1 Si1 102.57(7) 4_466 . ?
Si1 Ca1 Si1 116.82(3) 3_565 . ?
O1 Si1 O2 115.92(13) . . ?
O1 Si1 O3 116.18(12) . . ?
O2 Si1 O3 105.27(17) . . ?
O1 Si1 O4 107.67(17) . . ?
O2 Si1 O4 105.37(13) . . ?
O3 Si1 O4 105.47(12) . . ?
O1 Si1 Ca1 33.25(8) . 3_565 ?
O2 Si1 Ca1 89.73(9) . 3_565 ?
O3 Si1 Ca1 147.77(8) . 3_565 ?
O4 Si1 Ca1 97.48(10) . 3_565 ?
O1 Si1 Ca1 31.31(9) . . ?
O2 Si1 Ca1 144.66(7) . . ?
O3 Si1 Ca1 90.19(10) . . ?
O4 Si1 Ca1 100.59(14) . . ?
Ca1 Si1 Ca1 63.18(3) 3_565 . ?
O1 Si1 Ca1 95.75(12) . 3_665 ?
O2 Si1 Ca1 35.31(8) . 3_665 ?
O3 Si1 Ca1 91.08(13) . 3_665 ?
O4 Si1 Ca1 140.68(12) . 3_665 ?
Ca1 Si1 Ca1 84.98(3) 3_565 3_665 ?
Ca1 Si1 Ca1 115.04(3) . 3_665 ?
O1 Si1 Ca1 89.55(13) . 2_545 ?
O2 Si1 Ca1 139.01(9) . 2_545 ?
O3 Si1 Ca1 89.23(12) . 2_545 ?
O4 Si1 Ca1 33.81(11) . 2_545 ?
Ca1 Si1 Ca1 97.95(5) 3_565 2_545 ?
Ca1 Si1 Ca1 71.03(3) . 2_545 ?
Ca1 Si1 Ca1 173.92(3) 3_665 2_545 ?
O1 Si1 Ca1 151.82(9) . 2_645 ?
O2 Si1 Ca1 86.93(9) . 2_645 ?
O3 Si1 Ca1 37.40(7) . 2_645 ?
O4 Si1 Ca1 79.54(10) . 2_645 ?
Ca1 Si1 Ca1 174.75(2) 3_565 2_645 ?
Ca1 Si1 Ca1 121.48(3) . 2_645 ?
Ca1 Si1 Ca1 94.58(4) 3_665 2_645 ?
Ca1 Si1 Ca1 82.01(3) 2_545 2_645 ?
O1 Si1 Ca1 93.99(10) . 1_655 ?
O2 Si1 Ca1 89.12(11) . 1_655 ?
O3 Si1 Ca1 38.95(9) . 1_655 ?
O4 Si1 Ca1 144.41(8) . 1_655 ?
Ca1 Si1 Ca1 115.25(3) 3_565 1_655 ?
Ca1 Si1 Ca1 83.32(3) . 1_655 ?
Ca1 Si1 Ca1 60.39(3) 3_665 1_655 ?
Ca1 Si1 Ca1 122.32(3) 2_545 1_655 ?
Ca1 Si1 Ca1 68.78(2) 2_645 1_655 ?
O4 B1 O5 112.9(3) 3_655 . ?
O4 B1 O2 108.2(2) 3_655 . ?
O5 B1 O2 112.3(3) . . ?
O4 B1 O3 106.4(3) 3_655 4_565 ?
O5 B1 O3 110.0(2) . 4_565 ?
O2 B1 O3 106.6(3) . 4_565 ?
O4 B1 Ca1 117.5(3) 3_655 3_665 ?
O5 B1 Ca1 129.59(17) . 3_665 ?
O2 B1 Ca1 51.27(17) . 3_665 ?
O3 B1 Ca1 55.45(14) 4_565 3_665 ?
O4 B1 Ca1 49.6(2) 3_655 4_665 ?
O5 B1 Ca1 131.17(16) . 4_665 ?
O2 B1 Ca1 116.5(3) . 4_665 ?
O3 B1 Ca1 56.88(18) 4_565 4_665 ?
Ca1 B1 Ca1 84.65(13) 3_665 4_665 ?
Si1 O1 Ca1 124.24(13) . 3_565 ?
Si1 O1 Ca1 127.44(12) . . ?
Ca1 O1 Ca1 105.33(12) 3_565 . ?
B1 O2 Si1 120.5(3) . . ?
B1 O2 Ca1 99.6(2) . 3_665 ?
Si1 O2 Ca1 121.07(10) . 3_665 ?
B1 O3 Si1 120.6(3) 4_566 . ?
B1 O3 Ca1 94.85(14) 4_566 2_645 ?
Si1 O3 Ca1 118.78(10) . 2_645 ?
B1 O3 Ca1 93.40(17) 4_566 1_655 ?
Si1 O3 Ca1 116.78(11) . 1_655 ?
Ca1 O3 Ca1 107.90(12) 2_645 1_655 ?
B1 O4 Si1 126.0(3) 3_655 . ?
B1 O4 Ca1 101.9(2) 3_655 2_545 ?
Si1 O4 Ca1 123.00(12) . 2_545 ?
B1 O5 Ca1 119.09(18) . 4_565 ?
B1 O5 Ca1 119.66(16) . 3_565 ?
Ca1 O5 Ca1 106.41(10) 4_565 3_565 ?
B1 O5 H 99(7) . . ?
Ca1 O5 H 105(5) 4_565 . ?
Ca1 O5 H 106(5) 3_565 . ?

_refine_diff_density_max         1.434
_refine_diff_density_min         -1.655
_refine_diff_density_rms         0.336



# start Validation Reply Form
_vrf_PLAT029_shelx               
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.552 Why?  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT051_shelx               
;
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by .      80.45 %     
RESPONSE: ...
;
_vrf_PLAT250_shelx               
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        4.7 Note  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT911_shelx               
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        265 Report
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT926_shelx               
;
PROBLEM: Reported and Calculated   R1 Differ by .........    -0.0061 Check 
RESPONSE: ...
;
_vrf_PLAT973_shelx               
;
PROBLEM: Check Calcd Positive Resid. Density on       Ca1       1.99 eA-3  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC5
_database_code_depnum_ccdc_archive 'CCDC 1831443'
_audit_update_record             
;
2018-03-21 deposited with the CCDC.
2018-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B Ca H O5 Si'
_chemical_formula_weight         159.99

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0522 0.0431 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0004 0.0004 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.1611 0.1926 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   4.464(8)
_cell_length_b                   6.6986(9)
_cell_length_c                   9.2145(11)
_cell_angle_alpha                90
_cell_angle_beta                 90.76(3)
_cell_angle_gamma                90
_cell_volume                     275.5(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    621
_cell_measurement_theta_min      1.531
_cell_measurement_theta_max      11.935

_exptl_crystal_description       isosymmetric
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    3.857
_exptl_crystal_F_000             320
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.010
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.005
_exptl_absorpt_coefficient_mu    1.313
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.2896
_diffrn_radiation_type           ?
_diffrn_source                   ?
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            621
_diffrn_reflns_av_unetI/netI     0.0944
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.531
_diffrn_reflns_theta_max         11.935
_diffrn_reflns_theta_full        10.007
_diffrn_measured_fraction_theta_max 0.379
_diffrn_measured_fraction_theta_full 0.384
_diffrn_reflns_Laue_measured_fraction_max 0.379
_diffrn_reflns_Laue_measured_fraction_full 0.384
_diffrn_reflns_point_group_measured_fraction_max 0.379
_diffrn_reflns_point_group_measured_fraction_full 0.384
_reflns_number_total             320
_reflns_number_gt                241
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0867P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         320
_refine_ls_number_parameters     72
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0543
_refine_ls_wR_factor_ref         0.1406
_refine_ls_wR_factor_gt          0.1261
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_restrained_S_all      0.969
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca -0.0002(10) 0.62971(18) 0.18102(14) 0.024(2) Uani 1 1 d . . . . .
Si1 Si 0.5314(13) 0.3221(3) 0.06634(18) 0.018(3) Uani 1 1 d . . . . .
B1 B 0.592(7) 0.0574(12) -0.1516(9) 0.0061(16) Uiso 1 1 d . . . . .
O1 O 0.265(4) 0.4622(6) 0.0157(5) 0.032(9) Uani 1 1 d . . . . .
O2 O 0.728(4) 0.1767(7) -0.0378(5) 0.024(7) Uani 1 1 d . . . . .
O3 O 0.712(4) 0.3629(6) 0.2155(5) 0.032(9) Uani 1 1 d . . . . .
O4 O 0.309(3) 0.1405(6) 0.1313(5) 0.022(8) Uani 1 1 d . . . . .
O5 O 0.268(4) 0.0794(8) -0.1601(5) 0.015(10) Uani 1 1 d D . . . .
H H 0.088(19) 0.039(19) -0.13(2) 0.12(8) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O2 2.223(10) 3_665 ?
Ca1 O3 2.227(10) 1_455 ?
Ca1 O4 2.227(12) 2 ?
Ca1 O3 2.230(11) 2_655 ?
Ca1 O1 2.238(10) 3_565 ?
Ca1 O1 2.243(11) . ?
Ca1 O5 2.294(11) 3_565 ?
Ca1 O5 2.345(10) 4_566 ?
Ca1 B1 2.71(2) 4_466 ?
Ca1 B1 2.79(2) 3_665 ?
Ca1 Si1 3.110(6) 1_455 ?
Ca1 Si1 3.131(6) 3_665 ?
Si1 O1 1.580(14) . ?
Si1 O3 1.607(10) . ?
Si1 O2 1.632(11) . ?
Si1 O4 1.685(11) . ?
Si1 O1 1.871(11) 3_665 ?
Si1 Si1 2.691(4) 3_665 ?
Si1 Ca1 3.110(6) 1_655 ?
Si1 Ca1 3.131(6) 3_665 ?
Si1 Ca1 3.283(6) 3_565 ?
Si1 Ca1 3.366(5) 2_645 ?
Si1 Ca1 3.585(6) 2_545 ?
B1 O4 1.409(14) 3_655 ?
B1 O3 1.445(18) 4_565 ?
B1 O2 1.446(16) . ?
B1 O5 1.45(3) . ?
B1 Ca1 2.71(2) 4_665 ?
B1 Ca1 2.79(2) 3_665 ?
O1 Si1 1.871(11) 3_665 ?
O1 Ca1 2.238(10) 3_565 ?
O2 Ca1 2.223(10) 3_665 ?
O3 B1 1.445(18) 4_566 ?
O3 Ca1 2.227(10) 1_655 ?
O3 Ca1 2.230(10) 2_645 ?
O4 B1 1.409(14) 3_655 ?
O4 Ca1 2.227(12) 2_545 ?
O5 Ca1 2.294(11) 3_565 ?
O5 Ca1 2.345(10) 4_565 ?
O5 H 0.90(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ca1 O3 150.9(2) 3_665 1_455 ?
O2 Ca1 O4 142.3(2) 3_665 2 ?
O3 Ca1 O4 63.3(3) 1_455 2 ?
O2 Ca1 O3 61.9(3) 3_665 2_655 ?
O3 Ca1 O3 146.33(17) 1_455 2_655 ?
O4 Ca1 O3 90.3(4) 2 2_655 ?
O2 Ca1 O1 88.1(4) 3_665 3_565 ?
O3 Ca1 O1 66.1(3) 1_455 3_565 ?
O4 Ca1 O1 108.2(5) 2 3_565 ?
O3 Ca1 O1 146.6(2) 2_655 3_565 ?
O2 Ca1 O1 65.9(3) 3_665 . ?
O3 Ca1 O1 90.4(4) 1_455 . ?
O4 Ca1 O1 151.8(2) 2 . ?
O3 Ca1 O1 109.5(6) 2_655 . ?
O1 Ca1 O1 65.8(8) 3_565 . ?
O2 Ca1 O5 75.1(5) 3_665 3_565 ?
O3 Ca1 O5 113.1(6) 1_455 3_565 ?
O4 Ca1 O5 73.1(3) 2 3_565 ?
O3 Ca1 O5 74.9(5) 2_655 3_565 ?
O1 Ca1 O5 84.0(4) 3_565 3_565 ?
O1 Ca1 O5 130.4(2) . 3_565 ?
O2 Ca1 O5 116.1(6) 3_665 4_566 ?
O3 Ca1 O5 73.9(5) 1_455 4_566 ?
O4 Ca1 O5 81.5(4) 2 4_566 ?
O3 Ca1 O5 82.2(4) 2_655 4_566 ?
O1 Ca1 O5 127.0(2) 3_565 4_566 ?
O1 Ca1 O5 81.7(4) . 4_566 ?
O5 Ca1 O5 145.30(19) 3_565 4_566 ?
O2 Ca1 B1 169.9(6) 3_665 4_466 ?
O3 Ca1 B1 32.2(3) 1_455 4_466 ?
O4 Ca1 B1 31.3(3) 2 4_466 ?
O3 Ca1 B1 118.0(3) 2_655 4_466 ?
O1 Ca1 B1 89.0(5) 3_565 4_466 ?
O1 Ca1 B1 121.4(4) . 4_466 ?
O5 Ca1 B1 95.0(5) 3_565 4_466 ?
O5 Ca1 B1 73.1(5) 4_566 4_466 ?
O2 Ca1 B1 30.9(2) 3_665 3_665 ?
O3 Ca1 B1 174.2(6) 1_455 3_665 ?
O4 Ca1 B1 117.5(4) 2 3_665 ?
O3 Ca1 B1 30.9(2) 2_655 3_665 ?
O1 Ca1 B1 117.8(3) 3_565 3_665 ?
O1 Ca1 B1 87.6(5) . 3_665 ?
O5 Ca1 B1 72.2(5) 3_565 3_665 ?
O5 Ca1 B1 100.4(4) 4_566 3_665 ?
B1 Ca1 B1 147.9(3) 4_466 3_665 ?
O2 Ca1 Si1 123.7(2) 3_665 1_455 ?
O3 Ca1 Si1 29.55(19) 1_455 1_455 ?
O4 Ca1 Si1 82.2(3) 2 1_455 ?
O3 Ca1 Si1 172.2(4) 2_655 1_455 ?
O1 Ca1 Si1 36.6(2) 3_565 1_455 ?
O1 Ca1 Si1 78.3(4) . 1_455 ?
O5 Ca1 Si1 100.7(4) 3_565 1_455 ?
O5 Ca1 Si1 98.8(3) 4_566 1_455 ?
B1 Ca1 Si1 55.5(3) 4_466 1_455 ?
B1 Ca1 Si1 154.2(2) 3_665 1_455 ?
O2 Ca1 Si1 29.8(2) 3_665 3_665 ?
O3 Ca1 Si1 125.4(2) 1_455 3_665 ?
O4 Ca1 Si1 171.3(2) 2 3_665 ?
O3 Ca1 Si1 81.5(3) 2_655 3_665 ?
O1 Ca1 Si1 77.9(4) 3_565 3_665 ?
O1 Ca1 Si1 36.2(2) . 3_665 ?
O5 Ca1 Si1 101.8(3) 3_565 3_665 ?
O5 Ca1 Si1 100.1(4) 4_566 3_665 ?
B1 Ca1 Si1 157.3(2) 4_466 3_665 ?
B1 Ca1 Si1 53.8(3) 3_665 3_665 ?
Si1 Ca1 Si1 105.88(14) 1_455 3_665 ?
O1 Si1 O3 121.2(4) . . ?
O1 Si1 O2 126.1(4) . . ?
O3 Si1 O2 109.7(7) . . ?
O1 Si1 O4 95.1(7) . . ?
O3 Si1 O4 96.3(4) . . ?
O2 Si1 O4 95.8(5) . . ?
O1 Si1 O1 77.8(9) . 3_665 ?
O3 Si1 O1 88.5(5) . 3_665 ?
O2 Si1 O1 87.5(5) . 3_665 ?
O4 Si1 O1 172.9(7) . 3_665 ?
O1 Si1 Si1 42.8(5) . 3_665 ?
O3 Si1 Si1 106.6(2) . 3_665 ?
O2 Si1 Si1 108.4(3) . 3_665 ?
O4 Si1 Si1 137.9(6) . 3_665 ?
O1 Si1 Si1 35.0(5) 3_665 3_665 ?
O1 Si1 Ca1 101.9(4) . 1_655 ?
O3 Si1 Ca1 43.1(3) . 1_655 ?
O2 Si1 Ca1 103.4(6) . 1_655 ?
O4 Si1 Ca1 138.9(2) . 1_655 ?
O1 Si1 Ca1 45.4(3) 3_665 1_655 ?
Si1 Si1 Ca1 68.49(17) 3_665 1_655 ?
O1 Si1 Ca1 103.4(4) . 3_665 ?
O3 Si1 Ca1 105.8(6) . 3_665 ?
O2 Si1 Ca1 42.6(3) . 3_665 ?
O4 Si1 Ca1 137.3(3) . 3_665 ?
O1 Si1 Ca1 45.1(3) 3_665 3_665 ?
Si1 Si1 Ca1 69.19(17) 3_665 3_665 ?
Ca1 Si1 Ca1 74.12(14) 1_655 3_665 ?
O1 Si1 Ca1 37.2(2) . 3_565 ?
O3 Si1 Ca1 157.8(5) . 3_565 ?
O2 Si1 Ca1 92.3(4) . 3_565 ?
O4 Si1 Ca1 83.9(4) . 3_565 ?
O1 Si1 Ca1 89.6(4) 3_665 3_565 ?
Si1 Si1 Ca1 61.81(17) 3_665 3_565 ?
Ca1 Si1 Ca1 130.30(9) 1_655 3_565 ?
Ca1 Si1 Ca1 88.17(11) 3_665 3_565 ?
O1 Si1 Ca1 35.8(2) . . ?
O3 Si1 Ca1 88.5(5) . . ?
O2 Si1 Ca1 161.5(4) . . ?
O4 Si1 Ca1 84.7(4) . . ?
O1 Si1 Ca1 90.1(4) 3_665 . ?
Si1 Si1 Ca1 61.66(18) 3_665 . ?
Ca1 Si1 Ca1 87.76(12) 1_655 . ?
Ca1 Si1 Ca1 130.85(9) 3_665 . ?
Ca1 Si1 Ca1 69.38(13) 3_565 . ?
O1 Si1 Ca1 152.9(2) . 2_645 ?
O3 Si1 Ca1 34.3(3) . 2_645 ?
O2 Si1 Ca1 81.0(4) . 2_645 ?
O4 Si1 Ca1 80.9(4) . 2_645 ?
O1 Si1 Ca1 105.9(5) 3_665 2_645 ?
Si1 Si1 Ca1 135.5(3) 3_665 2_645 ?
Ca1 Si1 Ca1 67.03(11) 1_655 2_645 ?
Ca1 Si1 Ca1 97.3(2) 3_665 2_645 ?
Ca1 Si1 Ca1 162.63(10) 3_565 2_645 ?
Ca1 Si1 Ca1 117.20(10) . 2_645 ?
O1 Si1 Ca1 84.5(4) . 2_545 ?
O3 Si1 Ca1 80.4(5) . 2_545 ?
O2 Si1 Ca1 122.2(3) . 2_545 ?
O4 Si1 Ca1 27.4(2) . 2_545 ?
O1 Si1 Ca1 150.3(3) 3_665 2_545 ?
Si1 Si1 Ca1 123.2(3) 3_665 2_545 ?
Ca1 Si1 Ca1 117.71(10) 1_655 2_545 ?
Ca1 Si1 Ca1 164.57(6) 3_665 2_545 ?
Ca1 Si1 Ca1 90.5(2) 3_565 2_545 ?
Ca1 Si1 Ca1 62.32(11) . 2_545 ?
Ca1 Si1 Ca1 79.84(11) 2_645 2_545 ?
O4 B1 O3 110.0(15) 3_655 4_565 ?
O4 B1 O2 107.2(14) 3_655 . ?
O3 B1 O2 104.7(15) 4_565 . ?
O4 B1 O5 114.4(17) 3_655 . ?
O3 B1 O5 107.2(13) 4_565 . ?
O2 B1 O5 113.0(14) . . ?
O4 B1 Ca1 55.1(9) 3_655 4_665 ?
O3 B1 Ca1 55.2(9) 4_565 4_665 ?
O2 B1 Ca1 112.9(18) . 4_665 ?
O5 B1 Ca1 133.7(6) . 4_665 ?
O4 B1 Ca1 121.0(19) 3_655 3_665 ?
O3 B1 Ca1 52.5(8) 4_565 3_665 ?
O2 B1 Ca1 52.2(8) . 3_665 ?
O5 B1 Ca1 124.6(6) . 3_665 ?
Ca1 B1 Ca1 81.2(8) 4_665 3_665 ?
Si1 O1 Si1 102.2(9) . 3_665 ?
Si1 O1 Ca1 117.6(3) . 3_565 ?
Si1 O1 Ca1 98.0(2) 3_665 3_565 ?
Si1 O1 Ca1 119.9(3) . . ?
Si1 O1 Ca1 98.7(2) 3_665 . ?
Ca1 O1 Ca1 114.2(8) 3_565 . ?
B1 O2 Si1 122.2(16) . . ?
B1 O2 Ca1 96.9(8) . 3_665 ?
Si1 O2 Ca1 107.7(3) . 3_665 ?
B1 O3 Si1 126.9(16) 4_566 . ?
B1 O3 Ca1 92.6(8) 4_566 1_655 ?
Si1 O3 Ca1 107.3(3) . 1_655 ?
B1 O3 Ca1 96.6(8) 4_566 2_645 ?
Si1 O3 Ca1 121.8(3) . 2_645 ?
Ca1 O3 Ca1 107.0(7) 1_655 2_645 ?
B1 O4 Si1 122.8(16) 3_655 . ?
B1 O4 Ca1 93.6(10) 3_655 2_545 ?
Si1 O4 Ca1 132.3(3) . 2_545 ?
B1 O5 Ca1 127.5(7) . 3_565 ?
B1 O5 Ca1 118.2(6) . 4_565 ?
Ca1 O5 Ca1 101.1(6) 3_565 4_565 ?
B1 O5 H 148(10) . . ?
Ca1 O5 H 79(9) 3_565 . ?
Ca1 O5 H 64(10) 4_565 . ?

_refine_diff_density_max         0.628
_refine_diff_density_min         -0.634
_refine_diff_density_rms         0.162



# start Validation Reply Form
_vrf_PLAT029_shelx               
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.384 Why?  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT051_shelx               
;
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by .      81.70 %     
RESPONSE: ...
;
_vrf_PLAT088_shelx               
;
PROBLEM: Poor Data / Parameter Ratio ....................       4.44 Note  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT213_shelx               
;
PROBLEM: Atom O3              has ADP max/min Ratio .....        6.8 prolat
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT250_shelx               
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....       16.6 Note  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT911_shelx               
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        135 Report
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC6
_database_code_depnum_ccdc_archive 'CCDC 1831448'
_audit_update_record             
;
2018-03-21 deposited with the CCDC.
2018-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B Ca H O5 Si'
_chemical_formula_weight         159.99

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0522 0.0431 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0004 0.0004 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.1611 0.1926 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   4.538(3)
_cell_length_b                   6.7951(13)
_cell_length_c                   9.2277(9)
_cell_angle_alpha                90
_cell_angle_beta                 90.70(3)
_cell_angle_gamma                90
_cell_volume                     284.50(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1162
_cell_measurement_theta_min      2.240
_cell_measurement_theta_max      17.457

_exptl_crystal_description       isosymmetric
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    3.735
_exptl_crystal_F_000             320
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.010
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.005
_exptl_absorpt_coefficient_mu    1.272
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.2984
_diffrn_radiation_type           ?
_diffrn_source                   ?
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            1162
_diffrn_reflns_av_unetI/netI     0.0660
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.240
_diffrn_reflns_theta_max         17.457
_diffrn_reflns_theta_full        10.314
_diffrn_measured_fraction_theta_max 0.264
_diffrn_measured_fraction_theta_full 0.433
_diffrn_reflns_Laue_measured_fraction_max 0.264
_diffrn_reflns_Laue_measured_fraction_full 0.433
_diffrn_reflns_point_group_measured_fraction_max 0.264
_diffrn_reflns_point_group_measured_fraction_full 0.433
_reflns_number_total             640
_reflns_number_gt                477
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         640
_refine_ls_number_parameters     53
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1283
_refine_ls_R_factor_gt           0.1133
_refine_ls_wR_factor_ref         0.3172
_refine_ls_wR_factor_gt          0.2900
_refine_ls_goodness_of_fit_ref   1.200
_refine_ls_restrained_S_all      1.199
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca -0.0009(5) 0.63024(16) 0.18029(12) 0.0164(9) Uani 1 1 d . . . . .
Si1 Si 0.5281(7) 0.3205(2) 0.06630(18) 0.0140(11) Uani 1 1 d . . . . .
B1 B 0.587(3) 0.0577(8) -0.1524(6) 0.016(3) Uani 1 1 d . . . . .
O1 O 0.2618(19) 0.4610(6) 0.0170(4) 0.0141(11) Uani 1 1 d . . . . .
O2 O 0.724(2) 0.1802(6) -0.0398(5) 0.0141(11) Uani 1 1 d . . . . .
O3 O 0.7136(19) 0.3653(5) 0.2154(5) 0.0141(11) Uani 1 1 d . . . . .
O4 O 0.3162(18) 0.1388(6) 0.1313(5) 0.0141(11) Uani 1 1 d . . . . .
O5 O 0.2645(19) 0.0782(6) -0.1594(4) 0.0141(11) Uani 1 1 d D . . . .
H H 0.17(4) 0.01(2) -0.089(14) 0.07(6) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O2 2.226(8) 3_665 ?
Ca1 O3 2.244(6) 1_455 ?
Ca1 O1 2.247(5) 3_565 ?
Ca1 O1 2.249(7) . ?
Ca1 O4 2.266(8) 2 ?
Ca1 O3 2.268(5) 2_655 ?
Ca1 O5 2.321(6) 3_565 ?
Ca1 O5 2.367(5) 4_566 ?
Ca1 B1 2.753(12) 4_466 ?
Ca1 B1 2.846(10) 3_665 ?
Ca1 Si1 3.164(4) 3_665 ?
Ca1 Si1 3.170(3) 1_455 ?
Si1 O1 1.602(7) . ?
Si1 O3 1.633(5) . ?
Si1 O2 1.638(8) . ?
Si1 O4 1.680(7) . ?
Si1 O1 1.929(7) 3_665 ?
Si1 Si1 2.739(3) 3_665 ?
Si1 Ca1 3.164(4) 3_665 ?
Si1 Ca1 3.170(3) 1_655 ?
Si1 Ca1 3.299(3) 3_565 ?
Si1 Ca1 3.408(3) 2_645 ?
Si1 Ca1 3.606(4) 2_545 ?
B1 O4 1.418(8) 3_655 ?
B1 O3 1.452(11) 4_565 ?
B1 O2 1.464(7) . ?
B1 O5 1.471(16) . ?
B1 Ca1 2.753(12) 4_665 ?
B1 Ca1 2.846(10) 3_665 ?
O1 Si1 1.929(7) 3_665 ?
O1 Ca1 2.247(5) 3_565 ?
O2 Ca1 2.226(8) 3_665 ?
O3 B1 1.452(11) 4_566 ?
O3 Ca1 2.244(6) 1_655 ?
O3 Ca1 2.268(5) 2_645 ?
O4 B1 1.418(8) 3_655 ?
O4 Ca1 2.266(8) 2_545 ?
O5 Ca1 2.321(6) 3_565 ?
O5 Ca1 2.367(5) 4_565 ?
O5 H 0.90(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ca1 O3 151.54(17) 3_665 1_455 ?
O2 Ca1 O1 89.0(2) 3_665 3_565 ?
O3 Ca1 O1 66.19(19) 1_455 3_565 ?
O2 Ca1 O1 66.3(2) 3_665 . ?
O3 Ca1 O1 89.9(2) 1_455 . ?
O1 Ca1 O1 66.1(4) 3_565 . ?
O2 Ca1 O4 142.91(19) 3_665 2 ?
O3 Ca1 O4 62.5(2) 1_455 2 ?
O1 Ca1 O4 107.3(3) 3_565 2 ?
O1 Ca1 O4 150.70(18) . 2 ?
O2 Ca1 O3 60.94(18) 3_665 2_655 ?
O3 Ca1 O3 146.45(9) 1_455 2_655 ?
O1 Ca1 O3 146.35(18) 3_565 2_655 ?
O1 Ca1 O3 109.8(3) . 2_655 ?
O4 Ca1 O3 91.2(2) 2 2_655 ?
O2 Ca1 O5 75.6(3) 3_665 3_565 ?
O3 Ca1 O5 113.5(3) 1_455 3_565 ?
O1 Ca1 O5 84.39(19) 3_565 3_565 ?
O1 Ca1 O5 131.13(17) . 3_565 ?
O4 Ca1 O5 73.3(2) 2 3_565 ?
O3 Ca1 O5 74.2(2) 2_655 3_565 ?
O2 Ca1 O5 115.1(3) 3_665 4_566 ?
O3 Ca1 O5 73.7(2) 1_455 4_566 ?
O1 Ca1 O5 126.90(16) 3_565 4_566 ?
O1 Ca1 O5 80.96(19) . 4_566 ?
O4 Ca1 O5 81.8(2) 2 4_566 ?
O3 Ca1 O5 82.59(17) 2_655 4_566 ?
O5 Ca1 O5 145.14(11) 3_565 4_566 ?
O2 Ca1 B1 170.6(3) 3_665 4_466 ?
O3 Ca1 B1 31.8(2) 1_455 4_466 ?
O1 Ca1 B1 88.4(2) 3_565 4_466 ?
O1 Ca1 B1 120.5(2) . 4_466 ?
O4 Ca1 B1 30.93(17) 2 4_466 ?
O3 Ca1 B1 118.6(2) 2_655 4_466 ?
O5 Ca1 B1 95.1(3) 3_565 4_466 ?
O5 Ca1 B1 73.5(3) 4_566 4_466 ?
O2 Ca1 B1 30.54(16) 3_665 3_665 ?
O3 Ca1 B1 173.5(3) 1_455 3_665 ?
O1 Ca1 B1 118.3(2) 3_565 3_665 ?
O1 Ca1 B1 88.0(3) . 3_665 ?
O4 Ca1 B1 118.3(2) 2 3_665 ?
O3 Ca1 B1 30.40(19) 2_655 3_665 ?
O5 Ca1 B1 72.3(3) 3_565 3_665 ?
O5 Ca1 B1 99.9(3) 4_566 3_665 ?
B1 Ca1 B1 148.17(18) 4_466 3_665 ?
O2 Ca1 Si1 29.30(17) 3_665 3_665 ?
O3 Ca1 Si1 125.90(17) 1_455 3_665 ?
O1 Ca1 Si1 78.5(2) 3_565 3_665 ?
O1 Ca1 Si1 37.13(14) . 3_665 ?
O4 Ca1 Si1 171.55(13) 2 3_665 ?
O3 Ca1 Si1 80.77(19) 2_655 3_665 ?
O5 Ca1 Si1 101.73(18) 3_565 3_665 ?
O5 Ca1 Si1 99.7(2) 4_566 3_665 ?
B1 Ca1 Si1 157.42(14) 4_466 3_665 ?
B1 Ca1 Si1 53.30(19) 3_665 3_665 ?
O2 Ca1 Si1 125.01(13) 3_665 1_455 ?
O3 Ca1 Si1 29.20(11) 1_455 1_455 ?
O1 Ca1 Si1 37.01(16) 3_565 1_455 ?
O1 Ca1 Si1 78.39(19) . 1_455 ?
O4 Ca1 Si1 80.92(15) 2 1_455 ?
O3 Ca1 Si1 171.8(2) 2_655 1_455 ?
O5 Ca1 Si1 101.21(18) 3_565 1_455 ?
O5 Ca1 Si1 98.38(15) 4_566 1_455 ?
B1 Ca1 Si1 54.44(13) 4_466 1_455 ?
B1 Ca1 Si1 155.17(12) 3_665 1_455 ?
Si1 Ca1 Si1 106.97(8) 3_665 1_455 ?
O1 Si1 O3 120.5(3) . . ?
O1 Si1 O2 126.2(3) . . ?
O3 Si1 O2 109.5(4) . . ?
O1 Si1 O4 96.1(4) . . ?
O3 Si1 O4 97.3(3) . . ?
O2 Si1 O4 95.9(3) . . ?
O1 Si1 O1 78.7(5) . 3_665 ?
O3 Si1 O1 86.6(3) . 3_665 ?
O2 Si1 O1 86.3(3) . 3_665 ?
O4 Si1 O1 174.6(3) . 3_665 ?
O1 Si1 Si1 43.7(3) . 3_665 ?
O3 Si1 Si1 104.76(17) . 3_665 ?
O2 Si1 Si1 107.4(2) . 3_665 ?
O4 Si1 Si1 139.7(3) . 3_665 ?
O1 Si1 Si1 35.0(2) 3_665 3_665 ?
O1 Si1 Ca1 104.4(3) . 3_665 ?
O3 Si1 Ca1 103.8(3) . 3_665 ?
O2 Si1 Ca1 41.7(2) . 3_665 ?
O4 Si1 Ca1 136.9(2) . 3_665 ?
O1 Si1 Ca1 44.7(2) 3_665 3_665 ?
Si1 Si1 Ca1 69.20(12) 3_665 3_665 ?
O1 Si1 Ca1 101.7(2) . 1_655 ?
O3 Si1 Ca1 42.1(2) . 1_655 ?
O2 Si1 Ca1 102.5(3) . 1_655 ?
O4 Si1 Ca1 139.11(16) . 1_655 ?
O1 Si1 Ca1 44.52(13) 3_665 1_655 ?
Si1 Si1 Ca1 67.41(9) 3_665 1_655 ?
Ca1 Si1 Ca1 73.04(8) 3_665 1_655 ?
O1 Si1 Ca1 37.37(15) . 3_565 ?
O3 Si1 Ca1 157.6(3) . 3_565 ?
O2 Si1 Ca1 92.4(2) . 3_565 ?
O4 Si1 Ca1 84.7(2) . 3_565 ?
O1 Si1 Ca1 90.27(18) 3_665 3_565 ?
Si1 Si1 Ca1 62.53(8) 3_665 3_565 ?
Ca1 Si1 Ca1 89.17(6) 3_665 3_565 ?
Ca1 Si1 Ca1 129.94(6) 1_655 3_565 ?
O1 Si1 Ca1 34.77(19) . . ?
O3 Si1 Ca1 89.0(3) . . ?
O2 Si1 Ca1 160.8(2) . . ?
O4 Si1 Ca1 86.2(3) . . ?
O1 Si1 Ca1 90.1(2) 3_665 . ?
Si1 Si1 Ca1 61.35(11) 3_665 . ?
Ca1 Si1 Ca1 130.56(6) 3_665 . ?
Ca1 Si1 Ca1 87.81(6) 1_655 . ?
Ca1 Si1 Ca1 68.82(7) 3_565 . ?
O1 Si1 Ca1 152.5(2) . 2_645 ?
O3 Si1 Ca1 34.81(17) . 2_645 ?
O2 Si1 Ca1 81.22(19) . 2_645 ?
O4 Si1 Ca1 80.5(2) . 2_645 ?
O1 Si1 Ca1 104.8(2) 3_665 2_645 ?
Si1 Si1 Ca1 134.32(14) 3_665 2_645 ?
Ca1 Si1 Ca1 96.14(11) 3_665 2_645 ?
Ca1 Si1 Ca1 66.93(5) 1_655 2_645 ?
Ca1 Si1 Ca1 163.09(7) 3_565 2_645 ?
Ca1 Si1 Ca1 117.86(6) . 2_645 ?
O1 Si1 Ca1 83.9(3) . 2_545 ?
O3 Si1 Ca1 81.9(3) . 2_545 ?
O2 Si1 Ca1 123.3(2) . 2_545 ?
O4 Si1 Ca1 28.1(2) . 2_545 ?
O1 Si1 Ca1 150.4(2) 3_665 2_545 ?
Si1 Si1 Ca1 123.37(17) 3_665 2_545 ?
Ca1 Si1 Ca1 164.89(5) 3_665 2_545 ?
Ca1 Si1 Ca1 118.22(6) 1_655 2_545 ?
Ca1 Si1 Ca1 90.13(10) 3_565 2_545 ?
Ca1 Si1 Ca1 62.66(6) . 2_545 ?
Ca1 Si1 Ca1 80.56(6) 2_645 2_545 ?
O4 B1 O3 109.3(8) 3_655 4_565 ?
O4 B1 O2 108.0(6) 3_655 . ?
O3 B1 O2 102.8(7) 4_565 . ?
O4 B1 O5 113.7(7) 3_655 . ?
O3 B1 O5 109.4(6) 4_565 . ?
O2 B1 O5 113.0(8) . . ?
O4 B1 Ca1 55.2(5) 3_655 4_665 ?
O3 B1 Ca1 54.4(4) 4_565 4_665 ?
O2 B1 Ca1 112.1(8) . 4_665 ?
O5 B1 Ca1 134.6(3) . 4_665 ?
O4 B1 Ca1 120.7(8) 3_655 3_665 ?
O3 B1 Ca1 52.2(4) 4_565 3_665 ?
O2 B1 Ca1 50.6(4) . 3_665 ?
O5 B1 Ca1 125.6(4) . 3_665 ?
Ca1 B1 Ca1 80.9(4) 4_665 3_665 ?
Si1 O1 Si1 101.3(5) . 3_665 ?
Si1 O1 Ca1 117.0(3) . 3_565 ?
Si1 O1 Ca1 98.47(18) 3_665 3_565 ?
Si1 O1 Ca1 121.3(2) . . ?
Si1 O1 Ca1 98.2(2) 3_665 . ?
Ca1 O1 Ca1 113.9(4) 3_565 . ?
B1 O2 Si1 121.7(8) . . ?
B1 O2 Ca1 98.8(5) . 3_665 ?
Si1 O2 Ca1 109.0(2) . 3_665 ?
B1 O3 Si1 124.7(7) 4_566 . ?
B1 O3 Ca1 93.9(4) 4_566 1_655 ?
Si1 O3 Ca1 108.7(2) . 1_655 ?
B1 O3 Ca1 97.4(3) 4_566 2_645 ?
Si1 O3 Ca1 120.9(2) . 2_645 ?
Ca1 O3 Ca1 107.2(3) 1_655 2_645 ?
B1 O4 Si1 124.3(7) 3_655 . ?
B1 O4 Ca1 93.9(5) 3_655 2_545 ?
Si1 O4 Ca1 131.5(3) . 2_545 ?
B1 O5 Ca1 126.6(3) . 3_565 ?
B1 O5 Ca1 118.0(4) . 4_565 ?
Ca1 O5 Ca1 101.6(2) 3_565 4_565 ?
B1 O5 H 112(10) . . ?
Ca1 O5 H 105(10) 3_565 . ?
Ca1 O5 H 85(10) 4_565 . ?

_refine_diff_density_max         1.902
_refine_diff_density_min         -2.068
_refine_diff_density_rms         0.336



# start Validation Reply Form
_vrf_DIFMN02_shelx               
;
PROBLEM: The minimum difference density is < -0.1*ZMAX*1.00
RESPONSE: ...
;
_vrf_PLAT029_shelx               
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.433 Why?  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT051_shelx               
;
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by .      80.46 %     
RESPONSE: ...
;
_vrf_PLAT213_shelx               
;
PROBLEM: Atom B1              has ADP max/min Ratio .....        9.7 oblate
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT973_shelx               
;
PROBLEM: Check Calcd Positive Resid. Density on       Ca1       2.69 eA-3  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT098_shelx               
;
PROBLEM: Large Reported Min.  (Negative) Residual Density      -2.07 eA-3  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT250_shelx               
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        6.7 Note  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT911_shelx               
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        292 Report
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT926_shelx               
;
PROBLEM: Reported and Calculated   R1 Differ by .........    -0.0054 Check 
RESPONSE: ...
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC7
_database_code_depnum_ccdc_archive 'CCDC 1831442'
_audit_update_record             
;
2018-03-21 deposited with the CCDC.
2018-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B Ca H O5 Si'
_chemical_formula_weight         159.99

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0522 0.0431 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0004 0.0004 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.1611 0.1926 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   4.4367(19)
_cell_length_b                   7.2074(7)
_cell_length_c                   9.2808(5)
_cell_angle_alpha                90
_cell_angle_beta                 90.900(17)
_cell_angle_gamma                90
_cell_volume                     296.74(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1359
_cell_measurement_theta_min      1.502
_cell_measurement_theta_max      17.389

_exptl_crystal_description       isosymmetrical
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    3.581
_exptl_crystal_F_000             320
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.010
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.005
_exptl_absorpt_coefficient_mu    1.219
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.2984
_diffrn_radiation_type           ?
_diffrn_source                   ?
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            1359
_diffrn_reflns_av_unetI/netI     0.0600
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.502
_diffrn_reflns_theta_max         17.389
_diffrn_reflns_theta_full        10.314
_diffrn_measured_fraction_theta_max 0.290
_diffrn_measured_fraction_theta_full 0.517
_diffrn_reflns_Laue_measured_fraction_max 0.290
_diffrn_reflns_Laue_measured_fraction_full 0.517
_diffrn_reflns_point_group_measured_fraction_max 0.290
_diffrn_reflns_point_group_measured_fraction_full 0.517
_reflns_number_total             724
_reflns_number_gt                577
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         724
_refine_ls_number_parameters     47
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0847
_refine_ls_wR_factor_ref         0.2645
_refine_ls_wR_factor_gt          0.2347
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.0078(4) 0.60982(10) 0.17074(9) 0.0077(7) Uani 1 1 d . . . . .
Si1 Si 0.4897(6) 0.28081(16) 0.08052(13) 0.0063(8) Uani 1 1 d . . . . .
B1 B 0.588(2) 0.0838(5) -0.1561(6) 0.0064(7) Uiso 1 1 d . . . . .
O1 O 0.2508(15) 0.4241(4) 0.0294(4) 0.0092(9) Uani 1 1 d . . . . .
O2 O 0.7108(16) 0.1910(5) -0.0352(4) 0.0092(9) Uani 1 1 d . . . . .
O3 O 0.7086(15) 0.3407(5) 0.2138(4) 0.0092(9) Uani 1 1 d . . . . .
O4 O 0.3019(18) 0.1033(4) 0.1392(4) 0.0092(9) Uani 1 1 d . . . . .
O5 O 0.2602(16) 0.0919(4) -0.1597(4) 0.0092(9) Uani 1 1 d D . . . .
H H 0.17(2) 0.052(9) -0.080(6) 0.010 Uiso 1 1 d D U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O1 2.172(5) . ?
Ca1 O1 2.181(4) 3_565 ?
Ca1 O4 2.253(7) 2 ?
Ca1 O2 2.292(6) 3_665 ?
Ca1 O3 2.336(4) 2_655 ?
Ca1 O3 2.388(5) 1_455 ?
Ca1 O5 2.406(4) 4_566 ?
Ca1 O5 2.458(5) 3_565 ?
Ca1 B1 2.846(8) 4_466 ?
Ca1 B1 2.850(7) 3_665 ?
Ca1 Si1 3.282(2) 3_565 ?
Ca1 Si1 3.309(3) . ?
Si1 O1 1.549(5) . ?
Si1 O2 1.602(7) . ?
Si1 O3 1.619(4) . ?
Si1 O4 1.626(6) . ?
Si1 Ca1 3.282(2) 3_565 ?
Si1 Ca1 3.346(3) 3_665 ?
Si1 Ca1 3.398(2) 1_655 ?
Si1 Ca1 3.414(2) 2_645 ?
Si1 Ca1 3.447(3) 2_545 ?
B1 O3 1.436(9) 4_565 ?
B1 O4 1.442(6) 3_655 ?
B1 O5 1.454(12) . ?
B1 O2 1.461(6) . ?
B1 Ca1 2.846(8) 4_665 ?
B1 Ca1 2.850(7) 3_665 ?
O1 Ca1 2.181(4) 3_565 ?
O2 Ca1 2.292(6) 3_665 ?
O3 B1 1.436(9) 4_566 ?
O3 Ca1 2.336(4) 2_645 ?
O3 Ca1 2.388(5) 1_655 ?
O4 B1 1.442(6) 3_655 ?
O4 Ca1 2.253(7) 2_545 ?
O5 Ca1 2.406(4) 4_565 ?
O5 Ca1 2.458(5) 3_565 ?
O5 H 0.89(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ca1 O1 71.1(3) . 3_565 ?
O1 Ca1 O4 140.74(14) . 2 ?
O1 Ca1 O4 110.2(2) 3_565 2 ?
O1 Ca1 O2 77.0(2) . 3_665 ?
O1 Ca1 O2 83.49(19) 3_565 3_665 ?
O4 Ca1 O2 141.91(14) 2 3_665 ?
O1 Ca1 O3 116.6(2) . 2_655 ?
O1 Ca1 O3 137.97(14) 3_565 2_655 ?
O4 Ca1 O3 89.23(17) 2 2_655 ?
O2 Ca1 O3 60.77(14) 3_665 2_655 ?
O1 Ca1 O3 83.28(18) . 1_455 ?
O1 Ca1 O3 76.40(15) 3_565 1_455 ?
O4 Ca1 O3 60.30(15) 2 1_455 ?
O2 Ca1 O3 155.48(12) 3_665 1_455 ?
O3 Ca1 O3 143.01(8) 2_655 1_455 ?
O1 Ca1 O5 78.02(14) . 4_566 ?
O1 Ca1 O5 136.24(12) 3_565 4_566 ?
O4 Ca1 O5 76.04(19) 2 4_566 ?
O2 Ca1 O5 119.1(2) 3_665 4_566 ?
O3 Ca1 O5 83.60(14) 2_655 4_566 ?
O3 Ca1 O5 69.75(18) 1_455 4_566 ?
O1 Ca1 O5 139.28(13) . 3_565 ?
O1 Ca1 O5 79.33(14) 3_565 3_565 ?
O4 Ca1 O5 75.54(16) 2 3_565 ?
O2 Ca1 O5 72.3(2) 3_665 3_565 ?
O3 Ca1 O5 69.69(18) 2_655 3_565 ?
O3 Ca1 O5 116.6(2) 1_455 3_565 ?
O5 Ca1 O5 140.86(9) 4_566 3_565 ?
O1 Ca1 B1 111.99(17) . 4_466 ?
O1 Ca1 B1 94.9(2) 3_565 4_466 ?
O4 Ca1 B1 30.09(14) 2 4_466 ?
O2 Ca1 B1 169.9(2) 3_665 4_466 ?
O3 Ca1 B1 116.30(16) 2_655 4_466 ?
O3 Ca1 B1 30.27(14) 1_455 4_466 ?
O5 Ca1 B1 68.7(2) 4_566 4_466 ?
O5 Ca1 B1 97.6(2) 3_565 4_466 ?
O1 Ca1 B1 97.4(2) . 3_665 ?
O1 Ca1 B1 111.68(16) 3_565 3_665 ?
O4 Ca1 B1 116.48(17) 2 3_665 ?
O2 Ca1 B1 30.64(14) 3_665 3_665 ?
O3 Ca1 B1 30.13(16) 2_655 3_665 ?
O3 Ca1 B1 171.72(14) 1_455 3_665 ?
O5 Ca1 B1 102.26(19) 4_566 3_665 ?
O5 Ca1 B1 68.0(2) 3_565 3_665 ?
B1 Ca1 B1 145.63(12) 4_466 3_665 ?
O1 Ca1 Si1 93.06(12) . 3_565 ?
O1 Ca1 Si1 23.52(12) 3_565 3_565 ?
O4 Ca1 Si1 98.60(17) 2 3_565 ?
O2 Ca1 Si1 79.95(13) 3_665 3_565 ?
O3 Ca1 Si1 120.41(10) 2_655 3_565 ?
O3 Ca1 Si1 86.82(11) 1_455 3_565 ?
O5 Ca1 Si1 155.62(13) 4_566 3_565 ?
O5 Ca1 Si1 55.99(9) 3_565 3_565 ?
B1 Ca1 Si1 94.58(15) 4_466 3_565 ?
B1 Ca1 Si1 101.36(11) 3_665 3_565 ?
O1 Ca1 Si1 22.64(10) . . ?
O1 Ca1 Si1 92.15(15) 3_565 . ?
O4 Ca1 Si1 125.97(10) 2 . ?
O2 Ca1 Si1 87.15(15) 3_665 . ?
O3 Ca1 Si1 106.33(16) 2_655 . ?
O3 Ca1 Si1 79.82(14) 1_455 . ?
O5 Ca1 Si1 55.71(13) 4_566 . ?
O5 Ca1 Si1 158.46(15) 3_565 . ?
B1 Ca1 Si1 102.88(13) 4_466 . ?
B1 Ca1 Si1 97.66(17) 3_665 . ?
Si1 Ca1 Si1 114.98(5) 3_565 . ?
O1 Si1 O2 119.2(2) . . ?
O1 Si1 O3 117.1(2) . . ?
O2 Si1 O3 104.7(3) . . ?
O1 Si1 O4 106.0(3) . . ?
O2 Si1 O4 103.2(3) . . ?
O3 Si1 O4 105.0(2) . . ?
O1 Si1 Ca1 34.18(12) . 3_565 ?
O2 Si1 Ca1 91.90(16) . 3_565 ?
O3 Si1 Ca1 150.17(14) . 3_565 ?
O4 Si1 Ca1 94.87(19) . 3_565 ?
O1 Si1 Ca1 32.67(16) . . ?
O2 Si1 Ca1 149.76(13) . . ?
O3 Si1 Ca1 89.88(19) . . ?
O4 Si1 Ca1 98.2(3) . . ?
Ca1 Si1 Ca1 65.02(5) 3_565 . ?
O1 Si1 Ca1 95.1(2) . 3_665 ?
O2 Si1 Ca1 37.48(16) . 3_665 ?
O3 Si1 Ca1 94.1(2) . 3_665 ?
O4 Si1 Ca1 140.3(2) . 3_665 ?
Ca1 Si1 Ca1 84.05(4) 3_565 3_665 ?
Ca1 Si1 Ca1 116.60(5) . 3_665 ?
O1 Si1 Ca1 93.85(19) . 1_655 ?
O2 Si1 Ca1 91.6(2) . 1_655 ?
O3 Si1 Ca1 39.68(16) . 1_655 ?
O4 Si1 Ca1 144.58(14) . 1_655 ?
Ca1 Si1 Ca1 116.89(5) 3_565 1_655 ?
Ca1 Si1 Ca1 82.81(4) . 1_655 ?
Ca1 Si1 Ca1 63.37(5) 3_665 1_655 ?
O1 Si1 Ca1 152.16(14) . 2_645 ?
O2 Si1 Ca1 84.66(16) . 2_645 ?
O3 Si1 Ca1 37.08(13) . 2_645 ?
O4 Si1 Ca1 79.7(2) . 2_645 ?
Ca1 Si1 Ca1 172.72(4) 3_565 2_645 ?
Ca1 Si1 Ca1 120.34(5) . 2_645 ?
Ca1 Si1 Ca1 96.96(9) 3_665 2_645 ?
Ca1 Si1 Ca1 69.71(4) 1_655 2_645 ?
O1 Si1 Ca1 90.1(2) . 2_545 ?
O2 Si1 Ca1 135.20(16) . 2_545 ?
O3 Si1 Ca1 88.1(2) . 2_545 ?
O4 Si1 Ca1 32.55(19) . 2_545 ?
Ca1 Si1 Ca1 97.54(9) 3_565 2_545 ?
Ca1 Si1 Ca1 70.35(5) . 2_545 ?
Ca1 Si1 Ca1 172.68(5) 3_665 2_545 ?
Ca1 Si1 Ca1 121.49(5) 1_655 2_545 ?
Ca1 Si1 Ca1 80.58(4) 2_645 2_545 ?
O3 B1 O4 108.3(6) 4_565 3_655 ?
O3 B1 O5 110.6(5) 4_565 . ?
O4 B1 O5 112.2(5) 3_655 . ?
O3 B1 O2 107.8(5) 4_565 . ?
O4 B1 O2 106.8(4) 3_655 . ?
O5 B1 O2 111.0(6) . . ?
O3 B1 Ca1 56.9(3) 4_565 4_665 ?
O4 B1 Ca1 51.6(4) 3_655 4_665 ?
O5 B1 Ca1 132.0(3) . 4_665 ?
O2 B1 Ca1 116.9(6) . 4_665 ?
O3 B1 Ca1 54.7(3) 4_565 3_665 ?
O4 B1 Ca1 121.1(6) 3_655 3_665 ?
O5 B1 Ca1 126.7(3) . 3_665 ?
O2 B1 Ca1 53.1(3) . 3_665 ?
Ca1 B1 Ca1 86.2(3) 4_665 3_665 ?
Si1 O1 Ca1 124.7(2) . . ?
Si1 O1 Ca1 122.3(2) . 3_565 ?
Ca1 O1 Ca1 108.9(3) . 3_565 ?
B1 O2 Si1 120.2(6) . . ?
B1 O2 Ca1 96.3(4) . 3_665 ?
Si1 O2 Ca1 117.34(19) . 3_665 ?
B1 O3 Si1 121.0(6) 4_566 . ?
B1 O3 Ca1 95.1(3) 4_566 2_645 ?
Si1 O3 Ca1 118.22(18) . 2_645 ?
B1 O3 Ca1 92.8(3) 4_566 1_655 ?
Si1 O3 Ca1 114.66(18) . 1_655 ?
Ca1 O3 Ca1 111.0(2) 2_645 1_655 ?
B1 O4 Si1 126.7(7) 3_655 . ?
B1 O4 Ca1 98.3(4) 3_655 2_545 ?
Si1 O4 Ca1 124.6(2) . 2_545 ?
B1 O5 Ca1 116.5(3) . 4_565 ?
B1 O5 Ca1 121.2(3) . 3_565 ?
Ca1 O5 Ca1 106.3(2) 4_565 3_565 ?
B1 O5 H 116(6) . . ?
Ca1 O5 H 98(6) 4_565 . ?
Ca1 O5 H 95(5) 3_565 . ?

_refine_diff_density_max         1.833
_refine_diff_density_min         -1.331
_refine_diff_density_rms         0.332



# start Validation Reply Form
_vrf_PLAT029_shelx               
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.517 Why?  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT051_shelx               
;
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by .      80.45 %     
RESPONSE: ...
;
_vrf_PLAT250_shelx               
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        7.6 Note  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC8
_database_code_depnum_ccdc_archive 'CCDC 1831446'
_audit_update_record             
;
2018-03-21 deposited with the CCDC.
2018-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B Ca H O5 Si'
_chemical_formula_weight         159.99

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0522 0.0431 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0004 0.0004 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.1611 0.1926 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   4.531(4)
_cell_length_b                   6.6870(5)
_cell_length_c                   9.252(5)
_cell_angle_alpha                90
_cell_angle_beta                 90.27(8)
_cell_angle_gamma                90
_cell_volume                     280.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1057
_cell_measurement_theta_min      2.384
_cell_measurement_theta_max      17.324

_exptl_crystal_description       isosymmetric
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    3.791
_exptl_crystal_F_000             320
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.010
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.005
_exptl_absorpt_coefficient_mu    1.291
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.2896
_diffrn_radiation_type           ?
_diffrn_source                   ?
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            1057
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.384
_diffrn_reflns_theta_max         17.324
_diffrn_reflns_theta_full        10.007
_diffrn_measured_fraction_theta_max 0.203
_diffrn_measured_fraction_theta_full 0.338
_diffrn_reflns_Laue_measured_fraction_max 0.203
_diffrn_reflns_Laue_measured_fraction_full 0.338
_diffrn_reflns_point_group_measured_fraction_max 0.203
_diffrn_reflns_point_group_measured_fraction_full 0.338
_reflns_number_total             520
_reflns_number_gt                437
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1514P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.06(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         520
_refine_ls_number_parameters     54
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0415
_refine_ls_wR_factor_ref         0.1532
_refine_ls_wR_factor_gt          0.1372
_refine_ls_goodness_of_fit_ref   0.834
_refine_ls_restrained_S_all      0.833
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca -0.0003(4) 0.63078(8) 0.18039(16) 0.0088(12) Uani 1 1 d . . . . .
Si1 Si 0.5309(5) 0.32261(13) 0.0661(2) 0.0065(17) Uani 1 1 d . . . . .
B1 B 0.588(2) 0.0573(5) -0.1513(9) 0.007(5) Uani 1 1 d . . . . .
O1 O 0.2617(15) 0.4619(3) 0.0160(6) 0.008(2) Uani 1 1 d . . . . .
O2 O 0.7218(15) 0.1772(3) -0.0380(7) 0.008(2) Uani 1 1 d . . . . .
O3 O 0.7109(17) 0.3629(3) 0.2153(7) 0.008(2) Uani 1 1 d . . . . .
O4 O 0.3087(15) 0.1421(3) 0.1310(6) 0.008(2) Uani 1 1 d . . . . .
O5 O 0.2682(15) 0.0777(3) -0.1608(7) 0.008(2) Uani 1 1 d D . . . .
H H 0.20(3) 0.07(3) -0.069(6) 0.14(9) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O2 2.234(3) 3_665 ?
Ca1 O1 2.240(3) . ?
Ca1 O4 2.242(3) 2 ?
Ca1 O3 2.242(4) 1_455 ?
Ca1 O3 2.247(7) 2_655 ?
Ca1 O1 2.251(9) 3_565 ?
Ca1 O5 2.303(5) 3_565 ?
Ca1 O5 2.359(8) 4_566 ?
Ca1 B1 2.742(4) 4_466 ?
Ca1 B1 2.815(7) 3_665 ?
Ca1 Si1 3.139(3) 1_455 ?
Ca1 Si1 3.141(3) 3_665 ?
Si1 O1 1.601(7) . ?
Si1 O2 1.622(3) . ?
Si1 O3 1.623(10) . ?
Si1 O4 1.684(3) . ?
Si1 O1 1.882(3) 3_665 ?
Si1 Si1 2.683(3) 3_665 ?
Si1 Ca1 3.139(3) 1_655 ?
Si1 Ca1 3.141(3) 3_665 ?
Si1 Ca1 3.320(5) 3_565 ?
Si1 Ca1 3.409(4) 2_645 ?
Si1 Ca1 3.603(3) 2_545 ?
B1 O4 1.426(6) 3_655 ?
B1 O2 1.450(12) . ?
B1 O5 1.456(12) . ?
B1 O3 1.458(6) 4_565 ?
B1 Ca1 2.742(4) 4_665 ?
B1 Ca1 2.815(7) 3_665 ?
O1 Si1 1.882(3) 3_665 ?
O1 Ca1 2.251(9) 3_565 ?
O2 Ca1 2.234(3) 3_665 ?
O3 B1 1.458(6) 4_566 ?
O3 Ca1 2.242(4) 1_655 ?
O3 Ca1 2.247(7) 2_645 ?
O4 B1 1.426(6) 3_655 ?
O4 Ca1 2.242(3) 2_545 ?
O5 Ca1 2.303(5) 3_565 ?
O5 Ca1 2.359(8) 4_565 ?
O5 H 0.90(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ca1 O1 65.59(10) 3_665 . ?
O2 Ca1 O4 142.68(9) 3_665 2 ?
O1 Ca1 O4 151.64(9) . 2 ?
O2 Ca1 O3 151.1(2) 3_665 1_455 ?
O1 Ca1 O3 90.37(12) . 1_455 ?
O4 Ca1 O3 63.18(14) 2 1_455 ?
O2 Ca1 O3 61.7(2) 3_665 2_655 ?
O1 Ca1 O3 109.3(2) . 2_655 ?
O4 Ca1 O3 90.39(19) 2 2_655 ?
O3 Ca1 O3 146.07(12) 1_455 2_655 ?
O2 Ca1 O1 88.8(2) 3_665 3_565 ?
O1 Ca1 O1 65.9(3) . 3_565 ?
O4 Ca1 O1 108.1(3) 2 3_565 ?
O3 Ca1 O1 65.9(2) 1_455 3_565 ?
O3 Ca1 O1 147.20(16) 2_655 3_565 ?
O2 Ca1 O5 76.47(14) 3_665 3_565 ?
O1 Ca1 O5 130.87(18) . 3_565 ?
O4 Ca1 O5 72.69(14) 2 3_565 ?
O3 Ca1 O5 112.3(2) 1_455 3_565 ?
O3 Ca1 O5 75.8(3) 2_655 3_565 ?
O1 Ca1 O5 83.9(2) 3_565 3_565 ?
O2 Ca1 O5 114.6(2) 3_665 4_566 ?
O1 Ca1 O5 81.5(2) . 4_566 ?
O4 Ca1 O5 81.8(2) 2 4_566 ?
O3 Ca1 O5 74.8(3) 1_455 4_566 ?
O3 Ca1 O5 80.9(2) 2_655 4_566 ?
O1 Ca1 O5 127.43(17) 3_565 4_566 ?
O5 Ca1 O5 145.01(11) 3_565 4_566 ?
O2 Ca1 B1 170.5(2) 3_665 4_466 ?
O1 Ca1 B1 121.25(11) . 4_466 ?
O4 Ca1 B1 31.25(14) 2 4_466 ?
O3 Ca1 B1 32.07(16) 1_455 4_466 ?
O3 Ca1 B1 118.1(2) 2_655 4_466 ?
O1 Ca1 B1 88.6(3) 3_565 4_466 ?
O5 Ca1 B1 94.19(15) 3_565 4_466 ?
O5 Ca1 B1 74.1(2) 4_566 4_466 ?
O2 Ca1 B1 30.7(2) 3_665 3_665 ?
O1 Ca1 B1 87.38(14) . 3_665 ?
O4 Ca1 B1 117.78(16) 2 3_665 ?
O3 Ca1 B1 173.7(3) 1_455 3_665 ?
O3 Ca1 B1 31.0(2) 2_655 3_665 ?
O1 Ca1 B1 118.3(2) 3_565 3_665 ?
O5 Ca1 B1 73.5(2) 3_565 3_665 ?
O5 Ca1 B1 99.0(3) 4_566 3_665 ?
B1 Ca1 B1 148.05(10) 4_466 3_665 ?
O2 Ca1 Si1 124.2(2) 3_665 1_455 ?
O1 Ca1 Si1 78.47(18) . 1_455 ?
O4 Ca1 Si1 82.02(18) 2 1_455 ?
O3 Ca1 Si1 29.5(2) 1_455 1_455 ?
O3 Ca1 Si1 172.20(8) 2_655 1_455 ?
O1 Ca1 Si1 36.38(8) 3_565 1_455 ?
O5 Ca1 Si1 100.0(2) 3_565 1_455 ?
O5 Ca1 Si1 99.67(15) 4_566 1_455 ?
B1 Ca1 Si1 55.2(2) 4_466 1_455 ?
B1 Ca1 Si1 154.5(2) 3_665 1_455 ?
O2 Ca1 Si1 29.40(6) 3_665 3_665 ?
O1 Ca1 Si1 36.30(7) . 3_665 ?
O4 Ca1 Si1 171.24(14) 2 3_665 ?
O3 Ca1 Si1 125.55(9) 1_455 3_665 ?
O3 Ca1 Si1 81.23(9) 2_655 3_665 ?
O1 Ca1 Si1 78.28(11) 3_565 3_665 ?
O5 Ca1 Si1 102.55(7) 3_565 3_665 ?
O5 Ca1 Si1 99.31(10) 4_566 3_665 ?
B1 Ca1 Si1 157.35(10) 4_466 3_665 ?
B1 Ca1 Si1 53.47(10) 3_665 3_665 ?
Si1 Ca1 Si1 106.26(7) 1_455 3_665 ?
O1 Si1 O2 125.8(4) . . ?
O1 Si1 O3 121.9(3) . . ?
O2 Si1 O3 109.7(4) . . ?
O1 Si1 O4 93.7(3) . . ?
O2 Si1 O4 95.94(15) . . ?
O3 Si1 O4 96.6(3) . . ?
O1 Si1 O1 79.6(3) . 3_665 ?
O2 Si1 O1 87.18(13) . 3_665 ?
O3 Si1 O1 88.0(3) . 3_665 ?
O4 Si1 O1 173.2(4) . 3_665 ?
O1 Si1 Si1 43.63(13) . 3_665 ?
O2 Si1 Si1 108.32(16) . 3_665 ?
O3 Si1 Si1 106.95(14) . 3_665 ?
O4 Si1 Si1 137.3(3) . 3_665 ?
O1 Si1 Si1 35.9(2) 3_665 3_665 ?
O1 Si1 Ca1 103.2(2) . 1_655 ?
O2 Si1 Ca1 103.4(3) . 1_655 ?
O3 Si1 Ca1 42.92(10) . 1_655 ?
O4 Si1 Ca1 139.0(3) . 1_655 ?
O1 Si1 Ca1 45.2(3) 3_665 1_655 ?
Si1 Si1 Ca1 69.02(10) 3_665 1_655 ?
O1 Si1 Ca1 104.46(13) . 3_665 ?
O2 Si1 Ca1 42.55(9) . 3_665 ?
O3 Si1 Ca1 105.17(18) . 3_665 ?
O4 Si1 Ca1 137.55(11) . 3_665 ?
O1 Si1 Ca1 44.78(7) 3_665 3_665 ?
Si1 Si1 Ca1 69.57(4) 3_665 3_665 ?
Ca1 Si1 Ca1 73.74(7) 1_655 3_665 ?
O1 Si1 Ca1 36.7(2) . 3_565 ?
O2 Si1 Ca1 92.0(3) . 3_565 ?
O3 Si1 Ca1 158.14(16) . 3_565 ?
O4 Si1 Ca1 83.1(3) . 3_565 ?
O1 Si1 Ca1 90.7(3) 3_665 3_565 ?
Si1 Si1 Ca1 61.99(12) 3_665 3_565 ?
Ca1 Si1 Ca1 131.02(6) 1_655 3_565 ?
Ca1 Si1 Ca1 89.01(9) 3_665 3_565 ?
O1 Si1 Ca1 35.39(17) . . ?
O2 Si1 Ca1 160.8(3) . . ?
O3 Si1 Ca1 89.32(16) . . ?
O4 Si1 Ca1 84.06(14) . . ?
O1 Si1 Ca1 90.98(13) 3_665 . ?
Si1 Si1 Ca1 61.68(6) 3_665 . ?
Ca1 Si1 Ca1 88.61(6) 1_655 . ?
Ca1 Si1 Ca1 131.25(6) 3_665 . ?
Ca1 Si1 Ca1 68.87(8) 3_565 . ?
O1 Si1 Ca1 152.8(2) . 2_645 ?
O2 Si1 Ca1 81.4(3) . 2_645 ?
O3 Si1 Ca1 33.67(14) . 2_645 ?
O4 Si1 Ca1 81.8(3) . 2_645 ?
O1 Si1 Ca1 104.7(3) 3_665 2_645 ?
Si1 Si1 Ca1 135.20(15) 3_665 2_645 ?
Ca1 Si1 Ca1 66.19(8) 1_655 2_645 ?
Ca1 Si1 Ca1 96.57(9) 3_665 2_645 ?
Ca1 Si1 Ca1 162.77(5) 3_565 2_645 ?
Ca1 Si1 Ca1 117.51(8) . 2_645 ?
O1 Si1 Ca1 83.45(11) . 2_545 ?
O2 Si1 Ca1 122.19(10) . 2_545 ?
O3 Si1 Ca1 80.77(13) . 2_545 ?
O4 Si1 Ca1 27.24(10) . 2_545 ?
O1 Si1 Ca1 150.59(8) 3_665 2_545 ?
Si1 Si1 Ca1 122.89(9) 3_665 2_545 ?
Ca1 Si1 Ca1 117.83(7) 1_655 2_545 ?
Ca1 Si1 Ca1 164.61(4) 3_665 2_545 ?
Ca1 Si1 Ca1 89.85(9) 3_565 2_545 ?
Ca1 Si1 Ca1 61.97(5) . 2_545 ?
Ca1 Si1 Ca1 80.45(7) 2_645 2_545 ?
O4 B1 O2 106.6(8) 3_655 . ?
O4 B1 O5 115.0(5) 3_655 . ?
O2 B1 O5 113.9(3) . . ?
O4 B1 O3 109.1(3) 3_655 4_565 ?
O2 B1 O3 104.4(5) . 4_565 ?
O5 B1 O3 107.4(8) . 4_565 ?
O4 B1 Ca1 54.64(15) 3_655 4_665 ?
O2 B1 Ca1 112.3(5) . 4_665 ?
O5 B1 Ca1 133.5(6) . 4_665 ?
O3 B1 Ca1 54.7(2) 4_565 4_665 ?
O4 B1 Ca1 119.2(6) 3_655 3_665 ?
O2 B1 Ca1 51.9(2) . 3_665 ?
O5 B1 Ca1 125.8(3) . 3_665 ?
O3 B1 Ca1 52.5(4) 4_565 3_665 ?
Ca1 B1 Ca1 80.29(16) 4_665 3_665 ?
Si1 O1 Si1 100.4(3) . 3_665 ?
Si1 O1 Ca1 120.1(4) . . ?
Si1 O1 Ca1 98.92(12) 3_665 . ?
Si1 O1 Ca1 118.08(19) . 3_565 ?
Si1 O1 Ca1 98.5(3) 3_665 3_565 ?
Ca1 O1 Ca1 114.1(3) . 3_565 ?
B1 O2 Si1 122.5(5) . . ?
B1 O2 Ca1 97.3(3) . 3_665 ?
Si1 O2 Ca1 108.05(13) . 3_665 ?
B1 O3 Si1 126.0(7) 4_566 . ?
B1 O3 Ca1 93.2(3) 4_566 1_655 ?
Si1 O3 Ca1 107.6(2) . 1_655 ?
B1 O3 Ca1 96.5(6) 4_566 2_645 ?
Si1 O3 Ca1 122.72(14) . 2_645 ?
Ca1 O3 Ca1 105.9(4) 1_655 2_645 ?
B1 O4 Si1 121.4(5) 3_655 . ?
B1 O4 Ca1 94.11(18) 3_655 2_545 ?
Si1 O4 Ca1 132.66(19) . 2_545 ?
B1 O5 Ca1 127.4(2) . 3_565 ?
B1 O5 Ca1 119.5(3) . 4_565 ?
Ca1 O5 Ca1 100.4(3) 3_565 4_565 ?
B1 O5 H 105(10) . . ?
Ca1 O5 H 86(10) 3_565 . ?
Ca1 O5 H 114(10) 4_565 . ?

_refine_diff_density_max         0.495
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.137



# start Validation Reply Form
_vrf_PLAT029_shelx               
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.338 Why?  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT031_shelx               
;
PROBLEM: Refined Extinction Parameter Within Range ......      0.462 Sigma 
RESPONSE: ...
;
_vrf_PLAT051_shelx               
;
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by .      81.70 %     
RESPONSE: ...
;
_vrf_PLAT149_shelx               
;
PROBLEM: s.u. on the   beta    Angle is Too Large .......       0.08 Degree
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT911_shelx               
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        336 Report
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC9
_database_code_depnum_ccdc_archive 'CCDC 1831437'
_audit_update_record             
;
2018-03-21 deposited with the CCDC.
2018-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B Ca H O5 Si'
_chemical_formula_weight         159.99

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0522 0.0431 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0004 0.0004 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.1611 0.1926 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   4.579(3)
_cell_length_b                   7.2986(12)
_cell_length_c                   9.3814(15)
_cell_angle_alpha                90
_cell_angle_beta                 91.19(3)
_cell_angle_gamma                90
_cell_volume                     313.5(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1667
_cell_measurement_theta_min      1.484
_cell_measurement_theta_max      17.199

_exptl_crystal_description       isosymmetric
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    3.390
_exptl_crystal_F_000             320
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.010
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.005
_exptl_absorpt_coefficient_mu    1.154
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.2984
_diffrn_radiation_type           ?
_diffrn_source                   ?
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            1667
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.484
_diffrn_reflns_theta_max         17.199
_diffrn_reflns_theta_full        10.314
_diffrn_measured_fraction_theta_max 0.344
_diffrn_measured_fraction_theta_full 0.573
_diffrn_reflns_Laue_measured_fraction_max 0.344
_diffrn_reflns_Laue_measured_fraction_full 0.573
_diffrn_reflns_point_group_measured_fraction_max 0.344
_diffrn_reflns_point_group_measured_fraction_full 0.573
_reflns_number_total             878
_reflns_number_gt                792
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0988P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         878
_refine_ls_number_parameters     77
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0500
_refine_ls_wR_factor_ref         0.1635
_refine_ls_wR_factor_gt          0.1584
_refine_ls_goodness_of_fit_ref   1.282
_refine_ls_restrained_S_all      1.282
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.00472(19) 0.60989(6) 0.16920(5) 0.0096(3) Uani 1 1 d . . . . .
Si1 Si 0.4837(3) 0.27810(9) 0.08139(8) 0.0080(4) Uani 1 1 d . . . . .
B1 B 0.5806(11) 0.0840(3) -0.1550(3) 0.0097(10) Uani 1 1 d . . . . .
O1 O 0.2496(7) 0.4200(3) 0.0314(2) 0.0107(8) Uani 1 1 d . . . . .
O2 O 0.6999(8) 0.1940(2) -0.0376(2) 0.0081(7) Uani 1 1 d . . . . .
O3 O 0.6974(7) 0.3404(3) 0.2135(2) 0.0111(8) Uani 1 1 d . . . . .
O4 O 0.3045(8) 0.1002(2) 0.1413(2) 0.0106(8) Uani 1 1 d . . . . .
O5 O 0.2612(7) 0.0899(3) -0.1617(2) 0.0105(8) Uani 1 1 d D . . . .
H H 0.195(13) 0.044(5) -0.083(3) 0.009(11) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O1 2.204(2) 3_565 ?
Ca1 O1 2.216(3) . ?
Ca1 O4 2.297(4) 2 ?
Ca1 O2 2.339(3) 3_665 ?
Ca1 O3 2.417(2) 2_655 ?
Ca1 O5 2.438(2) 4_566 ?
Ca1 O3 2.459(3) 1_455 ?
Ca1 O5 2.507(2) 3_565 ?
Ca1 B1 2.937(4) 3_665 ?
Ca1 B1 2.937(4) 4_466 ?
Ca1 Si1 3.3132(16) 3_565 ?
Ca1 Si1 3.3806(16) . ?
Si1 O1 1.555(3) . ?
Si1 O2 1.628(3) . ?
Si1 O3 1.628(2) . ?
Si1 O4 1.641(3) . ?
Si1 Ca1 3.3132(17) 3_565 ?
Si1 Ca1 3.452(2) 3_665 ?
Si1 Ca1 3.4862(16) 1_655 ?
Si1 Ca1 3.4931(19) 2_545 ?
Si1 Ca1 3.4988(17) 2_645 ?
B1 O4 1.448(4) 3_655 ?
B1 O2 1.460(3) . ?
B1 O3 1.463(4) 4_565 ?
B1 O5 1.463(6) . ?
B1 Ca1 2.937(4) 3_665 ?
B1 Ca1 2.937(4) 4_665 ?
O1 Ca1 2.204(2) 3_565 ?
O2 Ca1 2.339(3) 3_665 ?
O3 B1 1.463(4) 4_566 ?
O3 Ca1 2.417(2) 2_645 ?
O3 Ca1 2.459(3) 1_655 ?
O4 B1 1.448(4) 3_655 ?
O4 Ca1 2.297(4) 2_545 ?
O5 Ca1 2.438(2) 4_565 ?
O5 Ca1 2.507(2) 3_565 ?
O5 H 0.87(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ca1 O1 72.83(12) 3_565 . ?
O1 Ca1 O4 109.56(12) 3_565 2 ?
O1 Ca1 O4 139.46(8) . 2 ?
O1 Ca1 O2 84.88(10) 3_565 3_665 ?
O1 Ca1 O2 76.69(11) . 3_665 ?
O4 Ca1 O2 143.12(7) 2 3_665 ?
O1 Ca1 O3 137.83(8) 3_565 2_655 ?
O1 Ca1 O3 114.42(11) . 2_655 ?
O4 Ca1 O3 91.15(9) 2 2_655 ?
O2 Ca1 O3 59.15(7) 3_665 2_655 ?
O1 Ca1 O5 137.35(7) 3_565 4_566 ?
O1 Ca1 O5 76.26(8) . 4_566 ?
O4 Ca1 O5 76.96(10) 2 4_566 ?
O2 Ca1 O5 115.68(11) 3_665 4_566 ?
O3 Ca1 O5 81.98(7) 2_655 4_566 ?
O1 Ca1 O3 76.77(8) 3_565 1_455 ?
O1 Ca1 O3 84.06(10) . 1_455 ?
O4 Ca1 O3 58.70(8) 2 1_455 ?
O2 Ca1 O3 156.62(7) 3_665 1_455 ?
O3 Ca1 O3 143.09(4) 2_655 1_455 ?
O5 Ca1 O3 71.41(9) 4_566 1_455 ?
O1 Ca1 O5 79.32(7) 3_565 3_565 ?
O1 Ca1 O5 141.43(8) . 3_565 ?
O4 Ca1 O5 75.03(9) 2 3_565 ?
O2 Ca1 O5 74.71(10) 3_665 3_565 ?
O3 Ca1 O5 70.95(9) 2_655 3_565 ?
O5 Ca1 O5 140.18(5) 4_566 3_565 ?
O3 Ca1 O5 115.12(11) 1_455 3_565 ?
O1 Ca1 B1 111.53(9) 3_565 3_665 ?
O1 Ca1 B1 96.54(12) . 3_665 ?
O4 Ca1 B1 117.91(9) 2 3_665 ?
O2 Ca1 B1 29.43(7) 3_665 3_665 ?
O3 Ca1 B1 29.74(8) 2_655 3_665 ?
O5 Ca1 B1 100.46(10) 4_566 3_665 ?
O3 Ca1 B1 171.51(7) 1_455 3_665 ?
O5 Ca1 B1 69.39(11) 3_565 3_665 ?
O1 Ca1 B1 95.06(11) 3_565 4_466 ?
O1 Ca1 B1 112.01(9) . 4_466 ?
O4 Ca1 B1 28.96(7) 2 4_466 ?
O2 Ca1 B1 170.92(10) 3_665 4_466 ?
O3 Ca1 B1 116.95(9) 2_655 4_466 ?
O5 Ca1 B1 70.22(11) 4_566 4_466 ?
O3 Ca1 B1 29.81(8) 1_455 4_466 ?
O5 Ca1 B1 96.34(11) 3_565 4_466 ?
B1 Ca1 B1 145.86(7) 3_665 4_466 ?
O1 Ca1 Si1 23.27(6) 3_565 3_565 ?
O1 Ca1 Si1 94.75(6) . 3_565 ?
O4 Ca1 Si1 97.98(9) 2 3_565 ?
O2 Ca1 Si1 82.16(7) 3_665 3_565 ?
O3 Ca1 Si1 121.17(5) 2_655 3_565 ?
O5 Ca1 Si1 156.65(6) 4_566 3_565 ?
O3 Ca1 Si1 86.39(6) 1_455 3_565 ?
O5 Ca1 Si1 56.23(5) 3_565 3_565 ?
B1 Ca1 Si1 101.97(7) 3_665 3_565 ?
B1 Ca1 Si1 94.19(8) 4_466 3_565 ?
O1 Ca1 Si1 93.16(8) 3_565 . ?
O1 Ca1 Si1 21.71(5) . . ?
O4 Ca1 Si1 125.46(6) 2 . ?
O2 Ca1 Si1 85.67(8) 3_665 . ?
O3 Ca1 Si1 104.29(8) 2_655 . ?
O5 Ca1 Si1 54.83(7) 4_566 . ?
O3 Ca1 Si1 81.06(8) 1_455 . ?
O5 Ca1 Si1 159.46(8) 3_565 . ?
B1 Ca1 Si1 96.35(9) 3_665 . ?
B1 Ca1 Si1 103.39(8) 4_466 . ?
Si1 Ca1 Si1 115.82(3) 3_565 . ?
O1 Si1 O2 118.01(13) . . ?
O1 Si1 O3 116.29(12) . . ?
O2 Si1 O3 105.23(16) . . ?
O1 Si1 O4 106.47(17) . . ?
O2 Si1 O4 104.62(13) . . ?
O3 Si1 O4 104.89(11) . . ?
O1 Si1 Ca1 34.04(8) . 3_565 ?
O2 Si1 Ca1 91.02(9) . 3_565 ?
O3 Si1 Ca1 149.03(8) . 3_565 ?
O4 Si1 Ca1 95.93(10) . 3_565 ?
O1 Si1 Ca1 31.80(9) . . ?
O2 Si1 Ca1 147.59(7) . . ?
O3 Si1 Ca1 89.84(10) . . ?
O4 Si1 Ca1 98.72(13) . . ?
Ca1 Si1 Ca1 64.18(3) 3_565 . ?
O1 Si1 Ca1 96.33(13) . 3_665 ?
O2 Si1 Ca1 35.99(8) . 3_665 ?
O3 Si1 Ca1 92.67(12) . 3_665 ?
O4 Si1 Ca1 140.53(11) . 3_665 ?
Ca1 Si1 Ca1 85.18(4) 3_565 3_665 ?
Ca1 Si1 Ca1 116.70(4) . 3_665 ?
O1 Si1 Ca1 94.17(10) . 1_655 ?
O2 Si1 Ca1 90.04(11) . 1_655 ?
O3 Si1 Ca1 39.51(9) . 1_655 ?
O4 Si1 Ca1 144.39(8) . 1_655 ?
Ca1 Si1 Ca1 116.41(3) 3_565 1_655 ?
Ca1 Si1 Ca1 83.63(4) . 1_655 ?
Ca1 Si1 Ca1 61.68(3) 3_665 1_655 ?
O1 Si1 Ca1 89.37(14) . 2_545 ?
O2 Si1 Ca1 137.23(8) . 2_545 ?
O3 Si1 Ca1 88.36(11) . 2_545 ?
O4 Si1 Ca1 32.96(10) . 2_545 ?
Ca1 Si1 Ca1 97.46(5) 3_565 2_545 ?
Ca1 Si1 Ca1 70.17(4) . 2_545 ?
Ca1 Si1 Ca1 173.03(3) 3_665 2_545 ?
Ca1 Si1 Ca1 122.03(3) 1_655 2_545 ?
O1 Si1 Ca1 151.96(8) . 2_645 ?
O2 Si1 Ca1 85.29(9) . 2_645 ?
O3 Si1 Ca1 37.38(8) . 2_645 ?
O4 Si1 Ca1 79.98(10) . 2_645 ?
Ca1 Si1 Ca1 173.58(2) 3_565 2_645 ?
Ca1 Si1 Ca1 121.14(3) . 2_645 ?
Ca1 Si1 Ca1 94.82(5) 3_665 2_645 ?
Ca1 Si1 Ca1 68.92(3) 1_655 2_645 ?
Ca1 Si1 Ca1 81.83(4) 2_545 2_645 ?
O4 B1 O2 108.3(2) 3_655 . ?
O4 B1 O3 106.6(3) 3_655 4_565 ?
O2 B1 O3 106.9(3) . 4_565 ?
O4 B1 O5 113.1(3) 3_655 . ?
O2 B1 O5 112.0(3) . . ?
O3 B1 O5 109.6(2) 4_565 . ?
O4 B1 Ca1 118.4(3) 3_655 3_665 ?
O2 B1 Ca1 51.94(17) . 3_665 ?
O3 B1 Ca1 55.02(14) 4_565 3_665 ?
O5 B1 Ca1 128.46(16) . 3_665 ?
O4 B1 Ca1 50.2(2) 3_655 4_665 ?
O2 B1 Ca1 116.6(3) . 4_665 ?
O3 B1 Ca1 56.68(17) 4_565 4_665 ?
O5 B1 Ca1 131.44(17) . 4_665 ?
Ca1 B1 Ca1 84.57(13) 3_665 4_665 ?
Si1 O1 Ca1 122.69(12) . 3_565 ?
Si1 O1 Ca1 126.49(12) . . ?
Ca1 O1 Ca1 107.17(12) 3_565 . ?
B1 O2 Si1 120.1(3) . . ?
B1 O2 Ca1 98.6(2) . 3_665 ?
Si1 O2 Ca1 119.87(10) . 3_665 ?
B1 O3 Si1 121.5(3) 4_566 . ?
B1 O3 Ca1 95.23(15) 4_566 2_645 ?
Si1 O3 Ca1 118.49(10) . 2_645 ?
B1 O3 Ca1 93.51(17) 4_566 1_655 ?
Si1 O3 Ca1 115.59(11) . 1_655 ?
Ca1 O3 Ca1 108.31(11) 2_645 1_655 ?
B1 O4 Si1 125.5(3) 3_655 . ?
B1 O4 Ca1 100.9(2) 3_655 2_545 ?
Si1 O4 Ca1 124.16(12) . 2_545 ?
B1 O5 Ca1 118.55(18) . 4_565 ?
B1 O5 Ca1 120.77(15) . 3_565 ?
Ca1 O5 Ca1 106.11(10) 4_565 3_565 ?
B1 O5 H 108(4) . . ?
Ca1 O5 H 98(3) 4_565 . ?
Ca1 O5 H 101(3) 3_565 . ?

_refine_diff_density_max         0.658
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.175



# start Validation Reply Form
_vrf_PLAT029_shelx               
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.573 Why?  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT051_shelx               
;
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by .      80.46 %     
RESPONSE: ...
;
_vrf_PLAT911_shelx               
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        244 Report
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC10
_database_code_depnum_ccdc_archive 'CCDC 1831445'
_audit_update_record             
;
2018-03-21 deposited with the CCDC.
2018-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B Ca H O5 Si'
_chemical_formula_weight         159.99

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   4.8347(10)
_cell_length_b                   7.6083(17)
_cell_length_c                   9.629(2)
_cell_angle_alpha                90
_cell_angle_beta                 90.230(4)
_cell_angle_gamma                90
_cell_volume                     354.17(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1516
_cell_measurement_theta_min      3.413
_cell_measurement_theta_max      35.709

_exptl_crystal_description       isosymmetric
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    3.000
_exptl_crystal_F_000             320
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.010
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.005
_exptl_absorpt_coefficient_mu    1.999
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX DUO CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            3886
_diffrn_reflns_av_unetI/netI     0.0620
_diffrn_reflns_av_R_equivalents  0.1044
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         3.413
_diffrn_reflns_theta_max         35.709
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             1516
_reflns_number_gt                1474
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0701P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.055(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1516
_refine_ls_number_parameters     78
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0397
_refine_ls_wR_factor_ref         0.1378
_refine_ls_wR_factor_gt          0.1278
_refine_ls_goodness_of_fit_ref   1.487
_refine_ls_restrained_S_all      1.486
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.00846(5) 0.60623(3) 0.16391(3) 0.00881(15) Uani 1 1 d . . . . .
Si1 Si 0.46900(7) 0.26614(5) 0.08434(4) 0.00662(16) Uani 1 1 d . . . . .
B1 B 0.5672(3) 0.08907(18) -0.15872(15) 0.0066(3) Uani 1 1 d . . . . .
O1 O 0.2402(2) 0.40085(13) 0.03734(12) 0.0099(2) Uani 1 1 d . . . . .
O2 O 0.6699(2) 0.19908(13) -0.04267(10) 0.0084(2) Uani 1 1 d . . . . .
O3 O 0.6754(2) 0.33464(14) 0.21028(10) 0.0088(2) Uani 1 1 d . . . . .
O4 O 0.3157(2) 0.08793(13) 0.14582(11) 0.0094(2) Uani 1 1 d . . . . .
O5 O 0.2584(2) 0.08639(14) -0.16364(12) 0.0100(2) Uani 1 1 d D . . . .
H H 0.188(6) 0.050(4) -0.082(2) 0.023(7) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O1 2.2768(12) 3_565 ?
Ca1 O1 2.2788(11) . ?
Ca1 O4 2.4198(12) 2 ?
Ca1 O2 2.4472(11) 3_665 ?
Ca1 O5 2.5198(11) 4_566 ?
Ca1 O3 2.6094(11) 2_655 ?
Ca1 O3 2.6586(11) 1_455 ?
Ca1 O5 2.6709(12) 3_565 ?
Ca1 B1 3.0961(15) 3_665 ?
Ca1 B1 3.1152(15) 4_466 ?
Ca1 Si1 3.4555(7) 3_565 ?
Ca1 Si1 3.5005(7) . ?
Si1 O1 1.5732(11) . ?
Si1 O2 1.6460(11) . ?
Si1 O3 1.6516(10) . ?
Si1 O4 1.6558(11) . ?
Si1 Ca1 3.4555(7) 3_565 ?
Si1 Ca1 3.5678(7) 2_545 ?
Si1 Ca1 3.6176(7) 3_665 ?
B1 O4 1.4659(17) 3_655 ?
B1 O2 1.4803(17) . ?
B1 O3 1.4854(18) 4_565 ?
B1 O5 1.4936(19) . ?
B1 Ca1 3.0962(15) 3_665 ?
B1 Ca1 3.1152(15) 4_665 ?
O1 Ca1 2.2768(12) 3_565 ?
O2 Ca1 2.4472(11) 3_665 ?
O3 B1 1.4854(18) 4_566 ?
O3 Ca1 2.6094(11) 2_645 ?
O3 Ca1 2.6586(11) 1_655 ?
O4 B1 1.4659(17) 3_655 ?
O4 Ca1 2.4197(12) 2_545 ?
O5 Ca1 2.5198(11) 4_565 ?
O5 Ca1 2.6709(12) 3_565 ?
O5 H 0.900(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ca1 O1 77.74(4) 3_565 . ?
O1 Ca1 O4 107.56(4) 3_565 2 ?
O1 Ca1 O4 133.37(4) . 2 ?
O1 Ca1 O2 86.71(4) 3_565 3_665 ?
O1 Ca1 O2 81.10(4) . 3_665 ?
O4 Ca1 O2 144.16(4) 2 3_665 ?
O1 Ca1 O5 142.87(4) 3_565 4_566 ?
O1 Ca1 O5 73.62(4) . 4_566 ?
O4 Ca1 O5 77.17(4) 2 4_566 ?
O2 Ca1 O5 111.25(4) 3_665 4_566 ?
O1 Ca1 O3 135.82(4) 3_565 2_655 ?
O1 Ca1 O3 114.62(4) . 2_655 ?
O4 Ca1 O3 93.83(4) 2 2_655 ?
O2 Ca1 O3 56.37(3) 3_665 2_655 ?
O5 Ca1 O3 78.63(4) 4_566 2_655 ?
O1 Ca1 O3 78.84(4) 3_565 1_455 ?
O1 Ca1 O3 81.74(4) . 1_455 ?
O4 Ca1 O3 55.50(3) 2 1_455 ?
O2 Ca1 O3 159.55(3) 3_665 1_455 ?
O5 Ca1 O3 74.13(3) 4_566 1_455 ?
O3 Ca1 O3 142.536(18) 2_655 1_455 ?
O1 Ca1 O5 76.50(3) 3_565 3_565 ?
O1 Ca1 O5 146.97(4) . 3_565 ?
O4 Ca1 O5 74.74(4) 2 3_565 ?
O2 Ca1 O5 77.14(4) 3_665 3_565 ?
O5 Ca1 O5 137.76(2) 4_566 3_565 ?
O3 Ca1 O5 72.51(3) 2_655 3_565 ?
O3 Ca1 O5 112.81(4) 1_455 3_565 ?
O1 Ca1 B1 110.59(4) 3_565 3_665 ?
O1 Ca1 B1 100.23(4) . 3_665 ?
O4 Ca1 B1 119.11(4) 2 3_665 ?
O2 Ca1 B1 27.97(4) 3_665 3_665 ?
O5 Ca1 B1 97.47(4) 4_566 3_665 ?
O3 Ca1 B1 28.59(4) 2_655 3_665 ?
O3 Ca1 B1 170.57(3) 1_455 3_665 ?
O5 Ca1 B1 70.40(4) 3_565 3_665 ?
O1 Ca1 B1 95.44(4) 3_565 4_466 ?
O1 Ca1 B1 107.78(4) . 4_466 ?
O4 Ca1 B1 27.18(4) 2 4_466 ?
O2 Ca1 B1 171.11(4) 3_665 4_466 ?
O5 Ca1 B1 71.88(4) 4_566 4_466 ?
O3 Ca1 B1 117.67(4) 2_655 4_466 ?
O3 Ca1 B1 28.43(3) 1_455 4_466 ?
O5 Ca1 B1 94.95(4) 3_565 4_466 ?
B1 Ca1 B1 145.21(3) 3_665 4_466 ?
O1 Ca1 Si1 21.41(3) 3_565 3_565 ?
O1 Ca1 Si1 98.70(3) . 3_565 ?
O4 Ca1 Si1 96.14(3) 2 3_565 ?
O2 Ca1 Si1 85.64(3) 3_665 3_565 ?
O5 Ca1 Si1 159.48(3) 4_566 3_565 ?
O3 Ca1 Si1 121.50(3) 2_655 3_565 ?
O3 Ca1 Si1 86.05(2) 1_455 3_565 ?
O5 Ca1 Si1 55.38(2) 3_565 3_565 ?
B1 Ca1 Si1 102.67(3) 3_665 3_565 ?
B1 Ca1 Si1 93.22(3) 4_466 3_565 ?
O1 Ca1 Si1 97.49(3) 3_565 . ?
O1 Ca1 Si1 20.21(3) . . ?
O4 Ca1 Si1 122.52(3) 2 . ?
O2 Ca1 Si1 86.40(3) 3_665 . ?
O5 Ca1 Si1 53.88(3) 4_566 . ?
O3 Ca1 Si1 102.82(3) 2_655 . ?
O3 Ca1 Si1 81.28(3) 1_455 . ?
O5 Ca1 Si1 162.69(3) 3_565 . ?
B1 Ca1 Si1 97.34(3) 3_665 . ?
B1 Ca1 Si1 101.83(3) 4_466 . ?
Si1 Ca1 Si1 118.689(14) 3_565 . ?
O1 Si1 O2 113.87(6) . . ?
O1 Si1 O3 115.32(6) . . ?
O2 Si1 O3 106.66(5) . . ?
O1 Si1 O4 108.73(6) . . ?
O2 Si1 O4 106.15(6) . . ?
O3 Si1 O4 105.42(6) . . ?
O1 Si1 Ca1 31.89(4) . 3_565 ?
O2 Si1 Ca1 88.16(4) . 3_565 ?
O3 Si1 Ca1 145.00(4) . 3_565 ?
O4 Si1 Ca1 100.29(4) . 3_565 ?
O1 Si1 Ca1 30.03(4) . . ?
O2 Si1 Ca1 140.32(4) . . ?
O3 Si1 Ca1 89.37(4) . . ?
O4 Si1 Ca1 103.95(4) . . ?
Ca1 Si1 Ca1 61.311(14) 3_565 . ?
O1 Si1 Ca1 87.79(5) . 2_545 ?
O2 Si1 Ca1 141.67(4) . 2_545 ?
O3 Si1 Ca1 89.96(4) . 2_545 ?
O4 Si1 Ca1 35.52(4) . 2_545 ?
Ca1 Si1 Ca1 97.675(19) 3_565 2_545 ?
Ca1 Si1 Ca1 71.913(14) . 2_545 ?
O1 Si1 Ca1 97.31(5) . 3_665 ?
O2 Si1 Ca1 34.56(4) . 3_665 ?
O3 Si1 Ca1 88.80(4) . 3_665 ?
O4 Si1 Ca1 140.42(4) . 3_665 ?
Ca1 Si1 Ca1 86.208(18) 3_565 3_665 ?
Ca1 Si1 Ca1 113.123(16) . 3_665 ?
Ca1 Si1 Ca1 174.795(13) 2_545 3_665 ?
O4 B1 O2 109.09(10) 3_655 . ?
O4 B1 O3 107.09(11) 3_655 4_565 ?
O2 B1 O3 107.57(10) . 4_565 ?
O4 B1 O5 112.07(11) 3_655 . ?
O2 B1 O5 111.34(11) . . ?
O3 B1 O5 109.49(10) 4_565 . ?
O4 B1 Ca1 115.69(8) 3_655 3_665 ?
O2 B1 Ca1 50.84(6) . 3_665 ?
O3 B1 Ca1 57.19(6) 4_565 3_665 ?
O5 B1 Ca1 132.22(8) . 3_665 ?
O4 B1 Ca1 48.95(6) 3_655 4_665 ?
O2 B1 Ca1 117.07(8) . 4_665 ?
O3 B1 Ca1 58.45(6) 4_565 4_665 ?
O5 B1 Ca1 131.51(9) . 4_665 ?
Ca1 B1 Ca1 83.86(4) 3_665 4_665 ?
Si1 O1 Ca1 126.70(6) . 3_565 ?
Si1 O1 Ca1 129.75(7) . . ?
Ca1 O1 Ca1 102.26(4) 3_565 . ?
B1 O2 Si1 122.61(9) . . ?
B1 O2 Ca1 101.19(8) . 3_665 ?
Si1 O2 Ca1 123.01(5) . 3_665 ?
B1 O3 Si1 122.21(8) 4_566 . ?
B1 O3 Ca1 94.22(7) 4_566 2_645 ?
Si1 O3 Ca1 118.80(5) . 2_645 ?
B1 O3 Ca1 93.12(7) 4_566 1_655 ?
Si1 O3 Ca1 119.11(5) . 1_655 ?
Ca1 O3 Ca1 103.97(4) 2_645 1_655 ?
B1 O4 Si1 127.54(9) 3_655 . ?
B1 O4 Ca1 103.87(8) 3_655 2_545 ?
Si1 O4 Ca1 121.05(6) . 2_545 ?
B1 O5 Ca1 120.37(8) . 4_565 ?
B1 O5 Ca1 118.09(8) . 3_565 ?
Ca1 O5 Ca1 106.15(4) 4_565 3_565 ?
B1 O5 H 111(2) . . ?
Ca1 O5 H 103(2) 4_565 . ?
Ca1 O5 H 95(2) 3_565 . ?

_refine_diff_density_max         1.081
_refine_diff_density_min         -1.075
_refine_diff_density_rms         0.183



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC11
_database_code_depnum_ccdc_archive 'CCDC 1831440'
_audit_update_record             
;
2018-03-21 deposited with the CCDC.
2018-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B Ca H O5 Si'
_chemical_formula_weight         159.99

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0522 0.0431 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0004 0.0004 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.1611 0.1926 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   4.7730(17)
_cell_length_b                   7.5294(6)
_cell_length_c                   9.5786(6)
_cell_angle_alpha                90
_cell_angle_beta                 90.442(14)
_cell_angle_gamma                90
_cell_volume                     344.23(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1857
_cell_measurement_theta_min      1.785
_cell_measurement_theta_max      17.466

_exptl_crystal_description       isosymmetric
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    3.087
_exptl_crystal_F_000             320
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.010
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.005
_exptl_absorpt_coefficient_mu    1.051
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.2984
_diffrn_radiation_type           ?
_diffrn_source                   ?
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            1857
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.785
_diffrn_reflns_theta_max         17.466
_diffrn_reflns_theta_full        10.314
_diffrn_measured_fraction_theta_max 0.285
_diffrn_measured_fraction_theta_full 0.462
_diffrn_reflns_Laue_measured_fraction_max 0.285
_diffrn_reflns_Laue_measured_fraction_full 0.462
_diffrn_reflns_point_group_measured_fraction_max 0.285
_diffrn_reflns_point_group_measured_fraction_full 0.462
_reflns_number_total             839
_reflns_number_gt                744
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0949P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       2.1(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         839
_refine_ls_number_parameters     78
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0424
_refine_ls_wR_factor_ref         0.1539
_refine_ls_wR_factor_gt          0.1204
_refine_ls_goodness_of_fit_ref   1.203
_refine_ls_restrained_S_all      1.202
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.0076(2) 0.60672(6) 0.16499(5) 0.0084(4) Uani 1 1 d . . . . .
Si1 Si 0.4736(3) 0.26857(9) 0.08393(7) 0.0072(5) Uani 1 1 d . . . . .
B1 B 0.5713(12) 0.0886(3) -0.1580(3) 0.0061(14) Uani 1 1 d . . . . .
O1 O 0.2446(9) 0.4051(2) 0.0359(2) 0.0099(11) Uani 1 1 d . . . . .
O2 O 0.6765(8) 0.1983(2) -0.04168(17) 0.0081(10) Uani 1 1 d . . . . .
O3 O 0.6809(8) 0.3360(2) 0.21110(18) 0.0079(10) Uani 1 1 d . . . . .
O4 O 0.3115(8) 0.0902(2) 0.1450(2) 0.0090(11) Uani 1 1 d . . . . .
O5 O 0.2587(8) 0.0882(3) -0.1635(2) 0.0100(12) Uani 1 1 d D . . . .
H H 0.204(18) 0.036(8) -0.085(4) 0.033(18) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O1 2.264(2) 3_565 ?
Ca1 O1 2.266(3) . ?
Ca1 O4 2.385(4) 2 ?
Ca1 O2 2.419(3) 3_665 ?
Ca1 O5 2.501(2) 4_566 ?
Ca1 O3 2.563(2) 2_655 ?
Ca1 O3 2.606(3) 1_455 ?
Ca1 O5 2.625(3) 3_565 ?
Ca1 B1 3.051(4) 3_665 ?
Ca1 B1 3.071(5) 4_466 ?
Ca1 Si1 3.4289(13) 3_565 ?
Ca1 Si1 3.4725(14) . ?
Si1 O1 1.566(3) . ?
Si1 O2 1.638(3) . ?
Si1 O3 1.644(2) . ?
Si1 O4 1.659(3) . ?
Si1 Ca1 3.4289(13) 3_565 ?
Si1 Ca1 3.5539(16) 2_545 ?
Si1 Ca1 3.5762(17) 3_665 ?
B1 O4 1.463(4) 3_655 ?
B1 O2 1.472(3) . ?
B1 O3 1.476(4) 4_565 ?
B1 O5 1.493(7) . ?
B1 Ca1 3.051(4) 3_665 ?
B1 Ca1 3.071(5) 4_665 ?
O1 Ca1 2.264(2) 3_565 ?
O2 Ca1 2.419(3) 3_665 ?
O3 B1 1.476(4) 4_566 ?
O3 Ca1 2.563(2) 2_645 ?
O3 Ca1 2.606(3) 1_655 ?
O4 B1 1.463(4) 3_655 ?
O4 Ca1 2.385(4) 2_545 ?
O5 Ca1 2.501(2) 4_565 ?
O5 Ca1 2.625(3) 3_565 ?
O5 H 0.89(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ca1 O1 76.97(13) 3_565 . ?
O1 Ca1 O4 107.93(14) 3_565 2 ?
O1 Ca1 O4 134.89(9) . 2 ?
O1 Ca1 O2 86.45(10) 3_565 3_665 ?
O1 Ca1 O2 79.90(11) . 3_665 ?
O4 Ca1 O2 143.92(7) 2 3_665 ?
O1 Ca1 O5 141.63(7) 3_565 4_566 ?
O1 Ca1 O5 74.12(8) . 4_566 ?
O4 Ca1 O5 76.94(11) 2 4_566 ?
O2 Ca1 O5 112.31(11) 3_665 4_566 ?
O1 Ca1 O3 136.28(7) 3_565 2_655 ?
O1 Ca1 O3 114.43(12) . 2_655 ?
O4 Ca1 O3 93.05(9) 2 2_655 ?
O2 Ca1 O3 57.04(7) 3_665 2_655 ?
O5 Ca1 O3 79.51(7) 4_566 2_655 ?
O1 Ca1 O3 78.37(9) 3_565 1_455 ?
O1 Ca1 O3 82.54(10) . 1_455 ?
O4 Ca1 O3 56.19(7) 2 1_455 ?
O2 Ca1 O3 158.98(6) 3_665 1_455 ?
O5 Ca1 O3 73.38(9) 4_566 1_455 ?
O3 Ca1 O3 142.54(4) 2_655 1_455 ?
O1 Ca1 O5 77.03(8) 3_565 3_565 ?
O1 Ca1 O5 145.81(7) . 3_565 ?
O4 Ca1 O5 74.78(9) 2 3_565 ?
O2 Ca1 O5 76.70(11) 3_665 3_565 ?
O5 Ca1 O5 138.27(5) 4_566 3_565 ?
O3 Ca1 O5 72.08(9) 2_655 3_565 ?
O3 Ca1 O5 113.26(12) 1_455 3_565 ?
O1 Ca1 B1 110.92(9) 3_565 3_665 ?
O1 Ca1 B1 99.21(13) . 3_665 ?
O4 Ca1 B1 118.72(8) 2 3_665 ?
O2 Ca1 B1 28.33(6) 3_665 3_665 ?
O5 Ca1 B1 98.23(10) 4_566 3_665 ?
O3 Ca1 B1 28.84(7) 2_655 3_665 ?
O3 Ca1 B1 170.71(6) 1_455 3_665 ?
O5 Ca1 B1 70.19(12) 3_565 3_665 ?
O1 Ca1 B1 95.28(12) 3_565 4_466 ?
O1 Ca1 B1 108.89(10) . 4_466 ?
O4 Ca1 B1 27.63(7) 2 4_466 ?
O2 Ca1 B1 171.20(8) 3_665 4_466 ?
O5 Ca1 B1 71.34(12) 4_566 4_466 ?
O3 Ca1 B1 117.41(8) 2_655 4_466 ?
O3 Ca1 B1 28.67(7) 1_455 4_466 ?
O5 Ca1 B1 95.25(11) 3_565 4_466 ?
B1 Ca1 B1 145.28(7) 3_665 4_466 ?
O1 Ca1 Si1 21.67(7) 3_565 3_565 ?
O1 Ca1 Si1 97.97(6) . 3_565 ?
O4 Ca1 Si1 96.69(8) 2 3_565 ?
O2 Ca1 Si1 84.89(7) 3_665 3_565 ?
O5 Ca1 Si1 158.77(7) 4_566 3_565 ?
O3 Ca1 Si1 121.37(5) 2_655 3_565 ?
O3 Ca1 Si1 86.19(6) 1_455 3_565 ?
O5 Ca1 Si1 55.60(5) 3_565 3_565 ?
B1 Ca1 Si1 102.52(6) 3_665 3_565 ?
B1 Ca1 Si1 93.53(8) 4_466 3_565 ?
O1 Ca1 Si1 96.81(8) 3_565 . ?
O1 Ca1 Si1 20.52(5) . . ?
O4 Ca1 Si1 123.11(6) 2 . ?
O2 Ca1 Si1 86.17(7) 3_665 . ?
O5 Ca1 Si1 54.00(7) 4_566 . ?
O3 Ca1 Si1 103.13(8) 2_655 . ?
O3 Ca1 Si1 81.34(8) 1_455 . ?
O5 Ca1 Si1 162.04(8) 3_565 . ?
B1 Ca1 Si1 97.08(10) 3_665 . ?
B1 Ca1 Si1 102.16(7) 4_466 . ?
Si1 Ca1 Si1 118.17(3) 3_565 . ?
O1 Si1 O2 114.30(13) . . ?
O1 Si1 O3 115.43(11) . . ?
O2 Si1 O3 106.74(18) . . ?
O1 Si1 O4 108.0(2) . . ?
O2 Si1 O4 106.12(13) . . ?
O3 Si1 O4 105.56(11) . . ?
O1 Si1 Ca1 32.25(7) . 3_565 ?
O2 Si1 Ca1 88.54(9) . 3_565 ?
O3 Si1 Ca1 145.78(8) . 3_565 ?
O4 Si1 Ca1 98.94(11) . 3_565 ?
O1 Si1 Ca1 30.46(8) . . ?
O2 Si1 Ca1 141.66(7) . . ?
O3 Si1 Ca1 89.48(11) . . ?
O4 Si1 Ca1 102.32(13) . . ?
Ca1 Si1 Ca1 61.83(3) 3_565 . ?
O1 Si1 Ca1 88.31(14) . 2_545 ?
O2 Si1 Ca1 140.82(8) . 2_545 ?
O3 Si1 Ca1 89.60(12) . 2_545 ?
O4 Si1 Ca1 34.71(10) . 2_545 ?
Ca1 Si1 Ca1 97.56(5) 3_565 2_545 ?
Ca1 Si1 Ca1 71.44(3) . 2_545 ?
O1 Si1 Ca1 96.73(14) . 3_665 ?
O2 Si1 Ca1 34.80(8) . 3_665 ?
O3 Si1 Ca1 89.83(13) . 3_665 ?
O4 Si1 Ca1 140.81(11) . 3_665 ?
Ca1 Si1 Ca1 85.87(3) 3_565 3_665 ?
Ca1 Si1 Ca1 113.86(3) . 3_665 ?
Ca1 Si1 Ca1 174.66(3) 2_545 3_665 ?
O4 B1 O2 108.9(3) 3_655 . ?
O4 B1 O3 106.8(3) 3_655 4_565 ?
O2 B1 O3 107.8(3) . 4_565 ?
O4 B1 O5 112.5(3) 3_655 . ?
O2 B1 O5 111.3(3) . . ?
O3 B1 O5 109.4(3) 4_565 . ?
O4 B1 Ca1 116.2(3) 3_655 3_665 ?
O2 B1 Ca1 51.23(17) . 3_665 ?
O3 B1 Ca1 56.92(15) 4_565 3_665 ?
O5 B1 Ca1 131.24(17) . 3_665 ?
O4 B1 Ca1 49.12(19) 3_655 4_665 ?
O2 B1 Ca1 117.2(3) . 4_665 ?
O3 B1 Ca1 57.91(18) 4_565 4_665 ?
O5 B1 Ca1 131.42(15) . 4_665 ?
Ca1 B1 Ca1 84.16(14) 3_665 4_665 ?
Si1 O1 Ca1 126.08(12) . 3_565 ?
Si1 O1 Ca1 129.02(11) . . ?
Ca1 O1 Ca1 103.03(13) 3_565 . ?
B1 O2 Si1 122.5(3) . . ?
B1 O2 Ca1 100.4(2) . 3_665 ?
Si1 O2 Ca1 122.47(10) . 3_665 ?
B1 O3 Si1 122.2(3) 4_566 . ?
B1 O3 Ca1 94.24(14) 4_566 2_645 ?
Si1 O3 Ca1 118.61(10) . 2_645 ?
B1 O3 Ca1 93.42(18) 4_566 1_655 ?
Si1 O3 Ca1 118.26(10) . 1_655 ?
Ca1 O3 Ca1 105.05(12) 2_645 1_655 ?
B1 O4 Si1 126.6(3) 3_655 . ?
B1 O4 Ca1 103.2(2) 3_655 2_545 ?
Si1 O4 Ca1 121.97(12) . 2_545 ?
B1 O5 Ca1 119.87(19) . 4_565 ?
B1 O5 Ca1 118.83(16) . 3_565 ?
Ca1 O5 Ca1 106.29(10) 4_565 3_565 ?
B1 O5 H 106(6) . . ?
Ca1 O5 H 99(4) 4_565 . ?
Ca1 O5 H 105(5) 3_565 . ?

_refine_diff_density_max         0.616
_refine_diff_density_min         -0.837
_refine_diff_density_rms         0.155



# start Validation Reply Form
_vrf_PLAT029_shelx               
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.462 Why?  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT051_shelx               
;
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by .      80.46 %     
RESPONSE: ...
;
_vrf_PLAT213_shelx               
;
PROBLEM: Atom B1              has ADP max/min Ratio .....        4.4 oblate
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT911_shelx               
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        338 Report
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT934_shelx               
;
PROBLEM: Number of (Iobs-Icalc)/SigmaW > 10 Outliers ....          2 Check 
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC12
_database_code_depnum_ccdc_archive 'CCDC 1831447'
_audit_update_record             
;
2018-03-21 deposited with the CCDC.
2018-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B Ca H O5 Si'
_chemical_formula_weight         159.99

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0522 0.0431 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0004 0.0004 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.1611 0.1926 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   4.448(10)
_cell_length_b                   6.6725(7)
_cell_length_c                   9.1900(11)
_cell_angle_alpha                90
_cell_angle_beta                 90.73(4)
_cell_angle_gamma                90
_cell_volume                     272.7(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1054
_cell_measurement_theta_min      1.537
_cell_measurement_theta_max      17.468

_exptl_crystal_description       isosymmetric
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    3.896
_exptl_crystal_F_000             320
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.010
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.005
_exptl_absorpt_coefficient_mu    1.326
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.2896
_diffrn_radiation_type           ?
_diffrn_source                   ?
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            1054
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_h_max       2
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.537
_diffrn_reflns_theta_max         17.468
_diffrn_reflns_theta_full        10.007
_diffrn_measured_fraction_theta_max 0.192
_diffrn_measured_fraction_theta_full 0.321
_diffrn_reflns_Laue_measured_fraction_max 0.192
_diffrn_reflns_Laue_measured_fraction_full 0.321
_diffrn_reflns_point_group_measured_fraction_max 0.192
_diffrn_reflns_point_group_measured_fraction_full 0.321
_reflns_number_total             489
_reflns_number_gt                402
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1029P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         489
_refine_ls_number_parameters     48
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0495
_refine_ls_wR_factor_ref         0.1341
_refine_ls_wR_factor_gt          0.1224
_refine_ls_goodness_of_fit_ref   0.917
_refine_ls_restrained_S_all      0.916
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.0011(5) 0.62927(9) 0.18129(6) 0.0123(14) Uani 1 1 d . . . . .
Si1 Si 0.5328(7) 0.32237(13) 0.06600(9) 0.0109(18) Uani 1 1 d . . . . .
B1 B 0.594(3) 0.0579(4) -0.1512(4) 0.0058(5) Uiso 1 1 d . . . . .
O1 O 0.258(2) 0.4609(4) 0.0158(2) 0.011(2) Uani 1 1 d . . . . .
O2 O 0.729(2) 0.1766(3) -0.0372(2) 0.011(2) Uani 1 1 d . . . . .
O3 O 0.713(2) 0.3628(3) 0.2161(2) 0.011(2) Uani 1 1 d . . . . .
O4 O 0.3072(19) 0.1413(3) 0.1310(2) 0.011(2) Uani 1 1 d . . . . .
O5 O 0.2687(19) 0.0784(3) -0.1592(2) 0.011(2) Uani 1 1 d D . . . .
H H 0.17(2) 0.033(9) -0.080(6) 0.03(2) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O3 2.215(6) 2_655 ?
Ca1 O2 2.216(6) 3_665 ?
Ca1 O3 2.218(6) 1_455 ?
Ca1 O1 2.218(5) 3_565 ?
Ca1 O4 2.219(7) 2 ?
Ca1 O1 2.221(6) . ?
Ca1 O5 2.298(5) 3_565 ?
Ca1 O5 2.333(5) 4_566 ?
Ca1 B1 2.699(10) 4_466 ?
Ca1 B1 2.774(10) 3_665 ?
Ca1 Si1 3.098(4) 1_455 ?
Ca1 Si1 3.113(4) 3_665 ?
Si1 O1 1.595(9) . ?
Si1 O3 1.609(5) . ?
Si1 O2 1.621(6) . ?
Si1 O4 1.684(6) . ?
Si1 O1 1.880(6) 3_665 ?
Si1 Si1 2.6771(18) 3_665 ?
Si1 Ca1 3.098(4) 1_655 ?
Si1 Ca1 3.113(4) 3_665 ?
Si1 Ca1 3.282(5) 3_565 ?
Si1 Ca1 3.351(4) 2_645 ?
Si1 Ca1 3.582(5) 2_545 ?
B1 O4 1.412(6) 3_655 ?
B1 O3 1.436(8) 4_565 ?
B1 O2 1.440(7) . ?
B1 O5 1.453(15) . ?
B1 Ca1 2.699(10) 4_665 ?
B1 Ca1 2.774(10) 3_665 ?
B1 Ca1 3.283(12) 4_565 ?
O1 Si1 1.880(6) 3_665 ?
O1 Ca1 2.218(5) 3_565 ?
O2 Ca1 2.216(6) 3_665 ?
O3 B1 1.436(8) 4_566 ?
O3 Ca1 2.215(6) 2_645 ?
O3 Ca1 2.218(6) 1_655 ?
O4 B1 1.412(6) 3_655 ?
O4 Ca1 2.219(7) 2_545 ?
O5 Ca1 2.298(5) 3_565 ?
O5 Ca1 2.333(5) 4_565 ?
O5 H 0.90(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Ca1 O2 62.00(15) 2_655 3_665 ?
O3 Ca1 O3 146.38(9) 2_655 1_455 ?
O2 Ca1 O3 150.83(10) 3_665 1_455 ?
O3 Ca1 O1 145.95(12) 2_655 3_565 ?
O2 Ca1 O1 87.2(2) 3_665 3_565 ?
O3 Ca1 O1 66.70(16) 1_455 3_565 ?
O3 Ca1 O4 90.1(2) 2_655 2 ?
O2 Ca1 O4 142.01(12) 3_665 2 ?
O3 Ca1 O4 63.42(17) 1_455 2 ?
O1 Ca1 O4 108.9(3) 3_565 2 ?
O3 Ca1 O1 110.4(3) 2_655 . ?
O2 Ca1 O1 66.32(17) 3_665 . ?
O3 Ca1 O1 89.9(2) 1_455 . ?
O1 Ca1 O1 64.6(4) 3_565 . ?
O4 Ca1 O1 151.66(13) 2 . ?
O3 Ca1 O5 74.8(3) 2_655 3_565 ?
O2 Ca1 O5 74.8(3) 3_665 3_565 ?
O3 Ca1 O5 113.0(3) 1_455 3_565 ?
O1 Ca1 O5 83.82(19) 3_565 3_565 ?
O4 Ca1 O5 73.19(17) 2 3_565 ?
O1 Ca1 O5 129.94(12) . 3_565 ?
O3 Ca1 O5 82.20(18) 2_655 4_566 ?
O2 Ca1 O5 116.5(3) 3_665 4_566 ?
O3 Ca1 O5 74.0(3) 1_455 4_566 ?
O1 Ca1 O5 127.45(13) 3_565 4_566 ?
O4 Ca1 O5 81.3(2) 2 4_566 ?
O1 Ca1 O5 82.34(19) . 4_566 ?
O5 Ca1 O5 145.24(9) 3_565 4_566 ?
O3 Ca1 B1 117.99(18) 2_655 4_466 ?
O2 Ca1 B1 169.7(3) 3_665 4_466 ?
O3 Ca1 B1 32.11(13) 1_455 4_466 ?
O1 Ca1 B1 89.7(2) 3_565 4_466 ?
O4 Ca1 B1 31.49(12) 2 4_466 ?
O1 Ca1 B1 120.82(18) . 4_466 ?
O5 Ca1 B1 95.2(3) 3_565 4_466 ?
O5 Ca1 B1 73.0(3) 4_566 4_466 ?
O3 Ca1 B1 30.96(13) 2_655 3_665 ?
O2 Ca1 B1 31.05(12) 3_665 3_665 ?
O3 Ca1 B1 174.4(3) 1_455 3_665 ?
O1 Ca1 B1 117.05(17) 3_565 3_665 ?
O4 Ca1 B1 117.32(18) 2 3_665 ?
O1 Ca1 B1 88.3(3) . 3_665 ?
O5 Ca1 B1 72.0(3) 3_565 3_665 ?
O5 Ca1 B1 100.5(2) 4_566 3_665 ?
B1 Ca1 B1 147.88(14) 4_466 3_665 ?
O3 Ca1 Si1 172.2(2) 2_655 1_455 ?
O2 Ca1 Si1 123.27(12) 3_665 1_455 ?
O3 Ca1 Si1 29.77(9) 1_455 1_455 ?
O1 Ca1 Si1 36.95(13) 3_565 1_455 ?
O4 Ca1 Si1 82.55(18) 2 1_455 ?
O1 Ca1 Si1 77.4(2) . 1_455 ?
O5 Ca1 Si1 100.5(2) 3_565 1_455 ?
O5 Ca1 Si1 99.09(16) 4_566 1_455 ?
B1 Ca1 Si1 55.66(14) 4_466 1_455 ?
B1 Ca1 Si1 153.91(9) 3_665 1_455 ?
O3 Ca1 Si1 81.55(19) 2_655 3_665 ?
O2 Ca1 Si1 29.80(12) 3_665 3_665 ?
O3 Ca1 Si1 125.48(13) 1_455 3_665 ?
O1 Ca1 Si1 77.1(2) 3_565 3_665 ?
O4 Ca1 Si1 171.10(11) 2 3_665 ?
O1 Ca1 Si1 36.70(13) . 3_665 ?
O5 Ca1 Si1 101.50(16) 3_565 3_665 ?
O5 Ca1 Si1 100.4(2) 4_566 3_665 ?
B1 Ca1 Si1 157.33(9) 4_466 3_665 ?
B1 Ca1 Si1 53.80(15) 3_665 3_665 ?
Si1 Ca1 Si1 105.67(11) 1_455 3_665 ?
O1 Si1 O3 121.4(2) . . ?
O1 Si1 O2 126.5(2) . . ?
O3 Si1 O2 109.7(4) . . ?
O1 Si1 O4 93.5(4) . . ?
O3 Si1 O4 96.2(3) . . ?
O2 Si1 O4 96.0(3) . . ?
O1 Si1 O1 79.5(5) . 3_665 ?
O3 Si1 O1 88.3(3) . 3_665 ?
O2 Si1 O1 87.4(3) . 3_665 ?
O4 Si1 O1 173.0(4) . 3_665 ?
O1 Si1 Si1 43.7(2) . 3_665 ?
O3 Si1 Si1 106.87(12) . 3_665 ?
O2 Si1 Si1 108.81(14) . 3_665 ?
O4 Si1 Si1 137.2(3) . 3_665 ?
O1 Si1 Si1 35.9(3) 3_665 3_665 ?
O1 Si1 Ca1 103.0(2) . 1_655 ?
O3 Si1 Ca1 43.20(18) . 1_655 ?
O2 Si1 Ca1 103.4(3) . 1_655 ?
O4 Si1 Ca1 138.90(12) . 1_655 ?
O1 Si1 Ca1 45.18(14) 3_665 1_655 ?
Si1 Si1 Ca1 68.81(10) 3_665 1_655 ?
O1 Si1 Ca1 104.1(2) . 3_665 ?
O3 Si1 Ca1 106.3(3) . 3_665 ?
O2 Si1 Ca1 42.80(17) . 3_665 ?
O4 Si1 Ca1 137.61(15) . 3_665 ?
O1 Si1 Ca1 44.89(17) 3_665 3_665 ?
Si1 Si1 Ca1 69.33(10) 3_665 3_665 ?
Ca1 Si1 Ca1 74.33(11) 1_655 3_665 ?
O1 Si1 Ca1 36.70(11) . 3_565 ?
O3 Si1 Ca1 157.7(3) . 3_565 ?
O2 Si1 Ca1 92.5(2) . 3_565 ?
O4 Si1 Ca1 83.5(2) . 3_565 ?
O1 Si1 Ca1 90.2(2) 3_665 3_565 ?
Si1 Si1 Ca1 61.67(9) 3_665 3_565 ?
Ca1 Si1 Ca1 130.48(7) 1_655 3_565 ?
Ca1 Si1 Ca1 88.11(13) 3_665 3_565 ?
O1 Si1 Ca1 35.64(13) . . ?
O3 Si1 Ca1 88.4(3) . . ?
O2 Si1 Ca1 161.8(2) . . ?
O4 Si1 Ca1 84.2(2) . . ?
O1 Si1 Ca1 90.6(2) 3_665 . ?
Si1 Si1 Ca1 61.54(10) 3_665 . ?
Ca1 Si1 Ca1 87.80(13) 1_655 . ?
Ca1 Si1 Ca1 130.87(7) 3_665 . ?
Ca1 Si1 Ca1 69.36(11) 3_565 . ?
O1 Si1 Ca1 152.63(13) . 2_645 ?
O3 Si1 Ca1 34.27(15) . 2_645 ?
O2 Si1 Ca1 80.9(2) . 2_645 ?
O4 Si1 Ca1 81.1(2) . 2_645 ?
O1 Si1 Ca1 105.6(3) 3_665 2_645 ?
Si1 Si1 Ca1 135.83(14) 3_665 2_645 ?
Ca1 Si1 Ca1 67.03(9) 1_655 2_645 ?
Ca1 Si1 Ca1 97.69(16) 3_665 2_645 ?
Ca1 Si1 Ca1 162.47(6) 3_565 2_645 ?
Ca1 Si1 Ca1 117.00(8) . 2_645 ?
O1 Si1 Ca1 83.4(3) . 2_545 ?
O3 Si1 Ca1 80.3(3) . 2_545 ?
O2 Si1 Ca1 122.00(18) . 2_545 ?
O4 Si1 Ca1 27.07(13) . 2_545 ?
O1 Si1 Ca1 150.52(18) 3_665 2_545 ?
Si1 Si1 Ca1 122.89(17) 3_665 2_545 ?
Ca1 Si1 Ca1 117.67(8) 1_655 2_545 ?
Ca1 Si1 Ca1 164.55(3) 3_665 2_545 ?
Ca1 Si1 Ca1 90.26(15) 3_565 2_545 ?
Ca1 Si1 Ca1 62.17(9) . 2_545 ?
Ca1 Si1 Ca1 79.74(12) 2_645 2_545 ?
O4 B1 O3 109.9(7) 3_655 4_565 ?
O4 B1 O2 107.2(6) 3_655 . ?
O3 B1 O2 105.1(6) 4_565 . ?
O4 B1 O5 113.8(7) 3_655 . ?
O3 B1 O5 107.4(6) 4_565 . ?
O2 B1 O5 113.1(6) . . ?
O4 B1 Ca1 55.2(4) 3_655 4_665 ?
O3 B1 Ca1 55.2(4) 4_565 4_665 ?
O2 B1 Ca1 113.1(8) . 4_665 ?
O5 B1 Ca1 133.6(3) . 4_665 ?
O4 B1 Ca1 121.3(8) 3_655 3_665 ?
O3 B1 Ca1 52.5(3) 4_565 3_665 ?
O2 B1 Ca1 52.6(4) . 3_665 ?
O5 B1 Ca1 124.9(3) . 3_665 ?
Ca1 B1 Ca1 81.4(3) 4_665 3_665 ?
O4 B1 Ca1 87.2(5) 3_655 4_565 ?
O3 B1 Ca1 92.5(4) 4_565 4_565 ?
O2 B1 Ca1 151.2(7) . 4_565 ?
O5 B1 Ca1 38.7(2) . 4_565 ?
Ca1 B1 Ca1 95.59(16) 4_665 4_565 ?
Ca1 B1 Ca1 139.33(17) 3_665 4_565 ?
Si1 O1 Si1 100.5(5) . 3_665 ?
Si1 O1 Ca1 117.87(18) . 3_565 ?
Si1 O1 Ca1 97.87(12) 3_665 3_565 ?
Si1 O1 Ca1 119.62(15) . . ?
Si1 O1 Ca1 98.42(13) 3_665 . ?
Ca1 O1 Ca1 115.4(4) 3_565 . ?
B1 O2 Si1 122.2(8) . . ?
B1 O2 Ca1 96.4(4) . 3_665 ?
Si1 O2 Ca1 107.39(14) . 3_665 ?
B1 O3 Si1 127.3(8) 4_566 . ?
B1 O3 Ca1 96.5(3) 4_566 2_645 ?
Si1 O3 Ca1 121.59(15) . 2_645 ?
B1 O3 Ca1 92.7(4) 4_566 1_655 ?
Si1 O3 Ca1 107.03(17) . 1_655 ?
Ca1 O3 Ca1 107.2(4) 2_645 1_655 ?
B1 O4 Si1 122.4(8) 3_655 . ?
B1 O4 Ca1 93.3(4) 3_655 2_545 ?
Si1 O4 Ca1 132.73(15) . 2_545 ?
B1 O5 Ca1 127.0(3) . 3_565 ?
B1 O5 Ca1 118.4(3) . 4_565 ?
Ca1 O5 Ca1 100.8(3) 3_565 4_565 ?
B1 O5 H 114(7) . . ?
Ca1 O5 H 96(5) 3_565 . ?
Ca1 O5 H 94(6) 4_565 . ?

_refine_diff_density_max         0.830
_refine_diff_density_min         -0.680
_refine_diff_density_rms         0.156



# start Validation Reply Form
_vrf_PLAT029_shelx               
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.321 Why?  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT051_shelx               
;
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by .      81.69 %     
RESPONSE: ...
;
_vrf_PLAT250_shelx               
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        7.2 Note  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT911_shelx               
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        163 Report
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT927_shelx               
;
PROBLEM: Reported and Calculated  wR2 Differ by .........    -0.0052 Check 
RESPONSE: ...
;
# end Validation Reply Form
