# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 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_mo_170919a_a
_database_code_depnum_ccdc_archive 'CCDC 1870318'
_audit_update_record             
;
2018-09-28 deposited with the CCDC.
2018-12-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C2 H5 O6 P2 Sb'
_chemical_formula_weight         308.75

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -z'

_cell_length_a                   4.6984(3)
_cell_length_b                   4.9701(3)
_cell_length_c                   15.6294(10)
_cell_angle_alpha                83.332(2)
_cell_angle_beta                 83.799(2)
_cell_angle_gamma                68.098(2)
_cell_volume                     335.51(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6885
_cell_measurement_theta_min      3.95
_cell_measurement_theta_max      27.46

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.056
_exptl_crystal_F_000             292
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    4.567
_shelx_estimated_absorpt_T_min   0.740
_shelx_estimated_absorpt_T_max   0.875
_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      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8384
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.948
_diffrn_reflns_theta_max         27.494
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             1531
_reflns_number_gt                1378
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_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)+(0.0112P)²+2.7351P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1531
_refine_ls_number_parameters     104
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0383
_refine_ls_wR_factor_ref         0.0747
_refine_ls_wR_factor_gt          0.0717
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_restrained_S_all      1.156
_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
Sb1 Sb 0.00430(9) 0.32593(8) 0.73040(2) 0.01000(13) Uani 1 1 d . . . . .
P1 P 0.5862(3) -0.1616(3) 0.87027(10) 0.0117(3) Uani 1 1 d . . . . .
P2 P 0.4115(3) 0.7112(3) 0.62139(9) 0.0080(3) Uani 1 1 d . . . . .
H2 H 0.29(2) -0.37(2) 0.875(6) 0.04(3) Uiso 1 1 d . . . . .
O1 O 0.4369(12) -0.3959(10) 0.8933(3) 0.0215(10) Uani 1 1 d . . . . .
O2 O 0.9001(10) -0.3012(10) 0.8240(3) 0.0215(10) Uani 1 1 d . . . . .
O3 O 0.3730(11) 0.0983(9) 0.8204(3) 0.0224(10) Uani 1 1 d . . . . .
O4 O 0.7492(9) 0.6518(9) 0.6332(3) 0.0139(9) Uani 1 1 d . . . . .
O5 O 0.2048(10) 1.0275(8) 0.6333(3) 0.0148(9) Uani 1 1 d . . . . .
O6 O 0.3256(9) 0.4898(9) 0.6862(3) 0.0138(9) Uani 1 1 d . . . . .
C1 C 0.6485(13) -0.0658(12) 0.9713(4) 0.0123(12) Uani 1 1 d . . . . .
H1A H 0.784999 -0.238249 1.002217 0.015 Uiso 1 1 calc R U . . .
H1B H 0.750713 0.073404 0.960430 0.015 Uiso 1 1 calc R U . . .
C2 C 0.3802(13) 0.6432(12) 0.5141(3) 0.0106(11) Uani 1 1 d . . . . .
H2A H 0.176699 0.640931 0.509732 0.013 Uiso 1 1 calc R U . . .
H2B H 0.401327 0.801630 0.474689 0.013 Uiso 1 1 calc R 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
Sb1 O6 1.995(4) . ?
Sb1 O5 2.136(4) 1_545 ?
Sb1 O4 2.178(4) 1_455 ?
Sb1 O3 2.226(4) . ?
Sb1 O2 2.369(4) 1_465 ?
P1 O3 1.500(4) . ?
P1 O2 1.517(4) . ?
P1 O1 1.560(5) . ?
P1 C1 1.784(6) . ?
P2 O5 1.529(4) . ?
P2 O4 1.530(4) . ?
P2 O6 1.544(4) . ?
P2 C2 1.781(6) . ?
O1 H2 0.74(9) . ?
C1 C1 1.539(11) 2_657 ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C2 1.527(10) 2_666 ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?

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
O6 Sb1 O5 84.99(16) . 1_545 ?
O6 Sb1 O4 81.04(15) . 1_455 ?
O5 Sb1 O4 89.69(16) 1_545 1_455 ?
O6 Sb1 O3 77.86(16) . . ?
O5 Sb1 O3 94.39(17) 1_545 . ?
O4 Sb1 O3 158.06(15) 1_455 . ?
O6 Sb1 O2 78.80(16) . 1_465 ?
O5 Sb1 O2 163.73(15) 1_545 1_465 ?
O4 Sb1 O2 89.11(16) 1_455 1_465 ?
O3 Sb1 O2 80.98(17) . 1_465 ?
O3 P1 O2 114.2(3) . . ?
O3 P1 O1 110.1(3) . . ?
O2 P1 O1 108.8(3) . . ?
O3 P1 C1 110.7(3) . . ?
O2 P1 C1 107.0(3) . . ?
O1 P1 C1 105.6(3) . . ?
O5 P2 O4 112.5(2) . . ?
O5 P2 O6 113.5(2) . . ?
O4 P2 O6 105.4(2) . . ?
O5 P2 C2 107.2(2) . . ?
O4 P2 C2 108.6(2) . . ?
O6 P2 C2 109.6(3) . . ?
P1 O1 H2 118(7) . . ?
P1 O2 Sb1 122.3(2) . 1_645 ?
P1 O3 Sb1 154.8(3) . . ?
P2 O4 Sb1 122.0(2) . 1_655 ?
P2 O5 Sb1 141.9(3) . 1_565 ?
P2 O6 Sb1 146.5(3) . . ?
C1 C1 P1 113.7(5) 2_657 . ?
C1 C1 H1A 108.8 2_657 . ?
P1 C1 H1A 108.8 . . ?
C1 C1 H1B 108.8 2_657 . ?
P1 C1 H1B 108.8 . . ?
H1A C1 H1B 107.7 . . ?
C2 C2 P2 113.5(5) 2_666 . ?
C2 C2 H2A 108.9 2_666 . ?
P2 C2 H2A 108.9 . . ?
C2 C2 H2B 108.9 2_666 . ?
P2 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?

_refine_diff_density_max         1.068
_refine_diff_density_min         -1.092
_refine_diff_density_rms         0.256


_exptl_crystal_preparation       Luminescent
