# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_Compound1
_database_code_depnum_ccdc_archive 'CCDC 1417122'
_audit_update_record             
;
2015-08-05 deposited with the CCDC.
2016-03-24 downloaded from the CCDC.
;

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C3 H3 Mn O6 Rb'
_chemical_formula_sum            'C3 H3 Mn O6 Rb'
_chemical_formula_weight         275.46
_chemical_melting_point          ?
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rb Rb -0.9393 2.9676 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   11.2786(3)
_cell_length_b                   9.1088(3)
_cell_length_c                   7.0254(3)
_cell_angle_alpha                90
_cell_angle_beta                 96.6260(10)
_cell_angle_gamma                90
_cell_volume                     716.93(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    856
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    8.565
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  1.0
_exptl_absorpt_correction_T_max  1.3382
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    2.552
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.180
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.043
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_number            7071
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.456
_diffrn_reflns_theta_min         4.475
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                752
_reflns_number_total             822
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.650
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       0.0059(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     55
_refine_ls_number_reflns         822
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0232
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0069P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0526
_refine_ls_wR_factor_ref         0.0534
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C2-H2
 0.93 with sigma of 0.02
 O3-H2
 1.88 with sigma of 0.04
 This was done due to issues encountered with AFIX commands due to the C and H atoms involved being on special positions
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   ?
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
Rb1 Rb 0.5000 0.59590(3) 0.2500 0.01712(16) Uani 1 2 d S T P . .
Mn1 Mn 0.7500 0.7500 0.0000 0.01075(16) Uani 1 2 d S T P . .
O2 O 0.73637(14) 0.53462(18) 0.1317(2) 0.0193(4) Uani 1 1 d . . . . .
C1 C 0.8040(2) 0.4280(3) 0.1230(3) 0.0154(5) Uani 1 1 d . . . . .
H1 H 0.8475 0.4250 0.0183 0.018 Uiso 1 1 calc R . . . .
O1 O 0.82012(13) 0.32427(18) 0.2392(2) 0.0193(4) Uani 1 1 d . . . . .
O3 O 0.93418(14) 0.78681(19) 0.1204(2) 0.0188(4) Uani 1 1 d D . . . .
C2 C 1.0000 0.7233(4) 0.2500 0.0146(6) Uani 1 2 d DS T P . .
H2 H 1.0000 0.620(2) 0.2500 0.018 Uiso 1 2 d DRS T P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Rb1 0.0179(2) 0.0125(2) 0.0223(2) 0.000 0.00801(12) 0.000
Mn1 0.0104(3) 0.0090(3) 0.0124(3) 0.00118(16) -0.00075(17) -0.00053(16)
O2 0.0200(8) 0.0129(8) 0.0259(9) 0.0064(7) 0.0068(6) 0.0048(7)
C1 0.0186(11) 0.0153(11) 0.0130(11) 0.0013(9) 0.0047(8) 0.0010(9)
O1 0.0232(8) 0.0155(9) 0.0199(8) 0.0076(6) 0.0055(6) 0.0076(6)
O3 0.0143(7) 0.0233(9) 0.0179(8) 0.0032(7) -0.0027(6) -0.0033(7)
C2 0.0128(14) 0.0117(15) 0.0187(16) 0.000 -0.0004(11) 0.000

_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
Rb1 Rb1 3.9232(3) 5_665 ?
Rb1 Mn1 3.76141(13) 2_655 ?
Rb1 Mn1 3.76141(13) . ?
Rb1 O2 2.9363(15) . ?
Rb1 O2 2.9363(15) 2_655 ?
Rb1 O1 2.9005(15) 4_655 ?
Rb1 O1 2.9005(15) 3_455 ?
Rb1 O3 2.9850(17) 7_665 ?
Rb1 O3 3.0250(18) 4_645 ?
Rb1 O3 2.9850(17) 8_466 ?
Rb1 O3 3.0250(18) 3_445 ?
Rb1 C2 3.394(3) 3_445 ?
Mn1 Rb1 3.76141(13) 7_665 ?
Mn1 O2 2.1820(16) . ?
Mn1 O2 2.1819(16) 7_665 ?
Mn1 O1 2.1850(16) 6_565 ?
Mn1 O1 2.1850(16) 4_655 ?
Mn1 O3 2.1767(15) 7_665 ?
Mn1 O3 2.1767(15) . ?
O2 C1 1.241(3) . ?
C1 H1 0.9300 . ?
C1 O1 1.249(3) . ?
O1 Rb1 2.9005(15) 3_545 ?
O1 Mn1 2.1850(16) 4_645 ?
O3 Rb1 2.9850(17) 7_665 ?
O3 Rb1 3.0250(18) 3 ?
O3 C2 1.248(2) . ?
C2 O3 1.248(2) 2_755 ?
C2 H2 0.937(17) . ?

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
Mn1 Rb1 Rb1 131.430(2) 2_655 5_665 ?
Mn1 Rb1 Rb1 70.771(3) . 5_665 ?
Mn1 Rb1 Mn1 136.178(8) . 2_655 ?
O2 Rb1 Rb1 64.41(3) . 5_665 ?
O2 Rb1 Rb1 105.23(3) 2_655 5_665 ?
O2 Rb1 Mn1 163.17(3) 2_655 . ?
O2 Rb1 Mn1 35.38(3) 2_655 2_655 ?
O2 Rb1 Mn1 163.17(3) . 2_655 ?
O2 Rb1 Mn1 35.38(3) . . ?
O2 Rb1 O2 158.08(6) . 2_655 ?
O2 Rb1 O3 73.08(4) . 4_645 ?
O2 Rb1 O3 86.40(4) 2_655 4_645 ?
O2 Rb1 O3 129.80(4) . 8_466 ?
O2 Rb1 O3 73.08(4) 2_655 3_445 ?
O2 Rb1 O3 129.80(4) 2_655 7_665 ?
O2 Rb1 O3 59.73(4) . 7_665 ?
O2 Rb1 O3 86.40(4) . 3_445 ?
O2 Rb1 O3 59.73(4) 2_655 8_466 ?
O2 Rb1 C2 79.04(3) 2_655 3_445 ?
O2 Rb1 C2 79.04(3) . 3_445 ?
O1 Rb1 Rb1 111.61(3) 3_455 5_665 ?
O1 Rb1 Rb1 105.69(3) 4_655 5_665 ?
O1 Rb1 Mn1 35.40(3) 3_455 2_655 ?
O1 Rb1 Mn1 106.26(3) 3_455 . ?
O1 Rb1 Mn1 35.40(3) 4_655 . ?
O1 Rb1 Mn1 106.26(3) 4_655 2_655 ?
O1 Rb1 O2 59.24(4) 4_655 . ?
O1 Rb1 O2 59.24(4) 3_455 2_655 ?
O1 Rb1 O2 141.64(5) 4_655 2_655 ?
O1 Rb1 O2 141.64(5) 3_455 . ?
O1 Rb1 O1 88.36(7) 4_655 3_455 ?
O1 Rb1 O3 120.86(4) 3_455 3_445 ?
O1 Rb1 O3 61.48(4) 3_455 8_466 ?
O1 Rb1 O3 145.28(4) 4_655 3_445 ?
O1 Rb1 O3 87.94(4) 4_655 8_466 ?
O1 Rb1 O3 61.48(4) 4_655 7_665 ?
O1 Rb1 O3 87.94(4) 3_455 7_665 ?
O1 Rb1 O3 145.28(4) 3_455 4_645 ?
O1 Rb1 O3 120.86(4) 4_655 4_645 ?
O1 Rb1 C2 135.82(3) 4_655 3_445 ?
O1 Rb1 C2 135.82(3) 3_455 3_445 ?
O3 Rb1 Rb1 80.19(3) 4_645 5_665 ?
O3 Rb1 Rb1 49.69(3) 7_665 5_665 ?
O3 Rb1 Rb1 164.94(3) 8_466 5_665 ?
O3 Rb1 Rb1 48.81(3) 3_445 5_665 ?
O3 Rb1 Mn1 123.28(3) 8_466 . ?
O3 Rb1 Mn1 108.46(3) 4_645 . ?
O3 Rb1 Mn1 112.21(3) 3_445 . ?
O3 Rb1 Mn1 35.33(3) 8_466 2_655 ?
O3 Rb1 Mn1 35.33(3) 7_665 . ?
O3 Rb1 Mn1 123.28(3) 7_665 2_655 ?
O3 Rb1 Mn1 108.46(3) 3_445 2_655 ?
O3 Rb1 Mn1 112.21(3) 4_645 2_655 ?
O3 Rb1 O3 98.50(4) 7_665 3_445 ?
O3 Rb1 O3 121.22(5) 8_466 3_445 ?
O3 Rb1 O3 98.50(4) 8_466 4_645 ?
O3 Rb1 O3 121.22(5) 7_665 4_645 ?
O3 Rb1 O3 42.90(6) 3_445 4_645 ?
O3 Rb1 O3 138.06(7) 8_466 7_665 ?
O3 Rb1 C2 21.45(3) 4_645 3_445 ?
O3 Rb1 C2 110.97(3) 7_665 3_445 ?
O3 Rb1 C2 110.97(3) 8_466 3_445 ?
O3 Rb1 C2 21.45(3) 3_445 3_445 ?
C2 Rb1 Rb1 63.555(7) 3_445 5_665 ?
C2 Rb1 Mn1 111.911(4) 3_445 2_655 ?
C2 Rb1 Mn1 111.911(4) 3_445 . ?
Rb1 Mn1 Rb1 180.0 7_665 . ?
O2 Mn1 Rb1 128.81(4) 7_665 . ?
O2 Mn1 Rb1 51.19(4) . . ?
O2 Mn1 Rb1 128.81(4) . 7_665 ?
O2 Mn1 Rb1 51.19(4) 7_665 7_665 ?
O2 Mn1 O2 180.00(8) 7_665 . ?
O2 Mn1 O1 97.30(6) . 6_565 ?
O2 Mn1 O1 82.70(6) . 4_655 ?
O2 Mn1 O1 82.70(6) 7_665 6_565 ?
O2 Mn1 O1 97.30(6) 7_665 4_655 ?
O1 Mn1 Rb1 50.26(4) 6_565 7_665 ?
O1 Mn1 Rb1 129.74(4) 6_565 . ?
O1 Mn1 Rb1 50.26(4) 4_655 . ?
O1 Mn1 Rb1 129.74(4) 4_655 7_665 ?
O1 Mn1 O1 180.0 6_565 4_655 ?
O3 Mn1 Rb1 127.53(4) 7_665 7_665 ?
O3 Mn1 Rb1 127.53(4) . . ?
O3 Mn1 Rb1 52.47(4) 7_665 . ?
O3 Mn1 Rb1 52.47(4) . 7_665 ?
O3 Mn1 O2 85.15(6) . 7_665 ?
O3 Mn1 O2 94.85(6) 7_665 7_665 ?
O3 Mn1 O2 94.85(6) . . ?
O3 Mn1 O2 85.15(6) 7_665 . ?
O3 Mn1 O1 87.25(6) 7_665 4_655 ?
O3 Mn1 O1 92.75(6) 7_665 6_565 ?
O3 Mn1 O1 87.25(6) . 6_565 ?
O3 Mn1 O1 92.75(6) . 4_655 ?
O3 Mn1 O3 180.0 7_665 . ?
Mn1 O2 Rb1 93.43(5) . . ?
C1 O2 Rb1 138.26(15) . . ?
C1 O2 Mn1 127.53(15) . . ?
O2 C1 H1 116.4 . . ?
O2 C1 O1 127.2(2) . . ?
O1 C1 H1 116.4 . . ?
Mn1 O1 Rb1 94.35(5) 4_645 3_545 ?
C1 O1 Rb1 127.49(14) . 3_545 ?
C1 O1 Mn1 138.02(15) . 4_645 ?
Rb1 O3 Rb1 81.50(4) 7_665 3 ?
Mn1 O3 Rb1 92.20(5) . 7_665 ?
Mn1 O3 Rb1 116.77(7) . 3 ?
C2 O3 Rb1 96.15(16) . 3 ?
C2 O3 Rb1 127.94(10) . 7_665 ?
C2 O3 Mn1 132.27(15) . . ?
O3 C2 O3 124.8(3) . 2_755 ?
O3 C2 H2 117.60(15) . . ?
O3 C2 H2 117.60(15) 2_755 . ?

_shelx_res_file                  
;
    shelx.res created by SHELXL-2014/7

TITL shelx in C2/c #15
REM reset to C2/c #15
CELL 0.71073 11.2786 9.1088 7.0254 90 96.626 90
ZERR 4 0.0003 0.0003 0.0003 0 0.001 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C O Mn Rb H
UNIT 12 24 4 4 12
DFIX 0.93 C2 H2
DFIX 1.88 0.04 O3 H2

L.S. 10
PLAN  25
CONN 2 C2
BOND
MORE -1
BOND $H
CONF
fmap 2
acta
OMIT -1 1 1
OMIT 1 1 0
OMIT 2 0 0
OMIT 1 1 1
REM <olex2.extras>
REM <HklSrc "%.\\shelx.hkl">
REM </olex2.extras>

WGHT    0.006900
EXTI    0.005888
FVAR       0.26411
RB1   4    0.500000    0.595904    0.250000    10.50000    0.01785    0.01251 =
         0.02233    0.00000    0.00801    0.00000
MN1   3    0.750000    0.750000    0.000000    10.50000    0.01041    0.00902 =
         0.01235    0.00118   -0.00075   -0.00053
O2    2    0.736375    0.534617    0.131663    11.00000    0.02005    0.01292 =
         0.02593    0.00643    0.00680    0.00478
C1    1    0.803993    0.428010    0.122954    11.00000    0.01863    0.01531 =
         0.01296    0.00131    0.00468    0.00104
AFIX  43
H1    5    0.847458    0.425040    0.018292    11.00000   -1.20000
AFIX   0
O1    2    0.820123    0.324267    0.239211    11.00000    0.02320    0.01552 =
         0.01990    0.00764    0.00545    0.00757
O3    2    0.934185    0.786809    0.120419    11.00000    0.01429    0.02327 =
         0.01785    0.00317   -0.00265   -0.00330
C2    1    1.000000    0.723316    0.250000    10.50000    0.01277    0.01175 =
         0.01873    0.00000   -0.00045    0.00000
H2    5    1.000000    0.620444    0.250000    10.50000   -1.20000
HKLF 4

REM  shelx in C2/c #15
REM R1 =  0.0232 for     752 Fo > 4sig(Fo)  and  0.0264 for all     822 data
REM     55 parameters refined using      2 restraints

END

WGHT      0.0069      0.0000

REM Highest difference peak  0.650,  deepest hole -0.698,  1-sigma level  0.116
Q1    1   1.0000  0.4074  0.2500  10.50000  0.05    0.65
Q2    1   0.7446  0.4373 -0.0027  11.00000  0.05    0.63
Q3    1   0.5052  0.4807  0.1236  11.00000  0.05    0.45
Q4    1   0.7546  0.6313  0.1322  11.00000  0.05    0.45
Q5    1   0.4201  0.5157  0.1388  11.00000  0.05    0.44
Q6    1   0.4809  0.7083  0.1160  11.00000  0.05    0.42
Q7    1   0.5952  0.5437  0.1918  11.00000  0.05    0.36
Q8    1   0.6458  0.4200 -0.0006  11.00000  0.05    0.34
Q9    1   0.7790  0.8662  0.1251  11.00000  0.05    0.30
Q10   1   0.9154  0.8894  0.1475  11.00000  0.05    0.30
Q11   1   0.5851  0.4888  0.0388  11.00000  0.05    0.30
Q12   1   0.8331  0.5754  0.1549  11.00000  0.05    0.28
Q13   1   0.5809  0.5783  0.1153  11.00000  0.05    0.27
Q14   1   0.6741  0.5680  0.3652  11.00000  0.05    0.26
Q15   1   0.6577  0.5844  0.1282  11.00000  0.05    0.26
Q16   1   0.8726  0.5234  0.2488  11.00000  0.05    0.26
Q17   1   0.9111  0.4891  0.0222  11.00000  0.05    0.25
Q18   1   0.8941  0.8809  0.0021  11.00000  0.05    0.25
Q19   1   0.8486  0.9386  0.1519  11.00000  0.05    0.25
Q20   1   0.9212  0.4416 -0.1289  11.00000  0.05    0.25
Q21   1   0.7544  0.5423 -0.0987  11.00000  0.05    0.24
Q22   1   0.6783  0.5549  0.1568  11.00000  0.05    0.23
Q23   1   0.6762  0.4925 -0.0890  11.00000  0.05    0.23
Q24   1   0.5933  0.6594  0.1628  11.00000  0.05    0.23
Q25   1   1.0161  0.5215  0.1928  11.00000  0.05    0.22
;
_shelx_res_checksum              31907
_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_Compound2
_database_code_depnum_ccdc_archive 'CCDC 1417123'
_audit_update_record             
;
2015-08-05 deposited with the CCDC.
2016-03-24 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT430_Compound2           
;
PROBLEM: Short Inter D...A Contact  O1     ..  O1      ..       2.23 Ang.
RESPONSE: There are no hydrogen atoms missing in the structure - the atoms are both in the same formate ligand
;

# Added during the CSD deposition process: Wednesday 5th of August 2015 06:12:49 PM
# end Validation Reply Form


_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C3 H3 Co O6 Rb'
_chemical_formula_sum            'C3 H3 Co O6 Rb'
_chemical_formula_weight         279.45
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Rb Co C3 O6'
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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           182
_space_group_name_H-M_alt        'P 63 2 2'
_space_group_name_Hall           'P 6c 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'

_cell_length_a                   7.2350(3)
_cell_length_b                   7.2350(3)
_cell_length_c                   8.2926(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     375.92(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2067
_cell_measurement_temperature    149.98(19)
_cell_measurement_theta_max      28.9620
_cell_measurement_theta_min      4.0570
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    8.694
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71355
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.469
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       'hexagonal block'
_exptl_crystal_F_000             266
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3066
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.479
_diffrn_reflns_theta_min         3.251
_diffrn_ambient_temperature      149.98(19)
_diffrn_detector_area_resol_mean 10.4102
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -19.00   27.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -10.0626  -99.0000  -30.0000 46

#__ type_ start__ end____ width___ exp.time_
  2 omega  -14.00   42.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4923  -99.0000  -30.0000 56

#__ type_ start__ end____ width___ exp.time_
  3 omega   -6.00   85.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4923   38.0000 -120.0000 91

#__ type_ start__ end____ width___ exp.time_
  4 omega  -63.00   29.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4923  -57.0000   90.0000 92
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0539212000
_diffrn_orient_matrix_UB_12      0.0513192000
_diffrn_orient_matrix_UB_13      0.0721642000
_diffrn_orient_matrix_UB_21      -0.0925161000
_diffrn_orient_matrix_UB_22      0.0007034000
_diffrn_orient_matrix_UB_23      0.0274357000
_diffrn_orient_matrix_UB_31      -0.0367007000
_diffrn_orient_matrix_UB_32      -0.1008764000
_diffrn_orient_matrix_UB_33      0.0368547000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.406
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.898
_reflns_number_gt                323
_reflns_number_total             336
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.237
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details 
;
 Flack x determined using 90 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.008(9)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     19
_refine_ls_number_reflns         336
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0166
_refine_ls_R_factor_gt           0.0151
_refine_ls_restrained_S_all      1.119
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0156P)²+0.0103P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0319
_refine_ls_wR_factor_ref         0.0325
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   ?
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
Co1 Co 0.6667 0.3333 0.2500 0.00821(15) Uani 1 6 d S T P . .
Rb2 Rb 1.0000 0.0000 0.2500 0.01550(14) Uani 1 6 d S T P . .
O1 O 0.6929(2) 0.5856(2) 0.39300(14) 0.0142(3) Uani 1 1 d . . . . .
C1 C 0.5595(4) 0.5595(4) 0.5000 0.0177(6) Uani 1 2 d S T P . .
H1 H 0.4310 0.4310 0.5000 0.021 Uiso 1 2 calc RS T P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.00976(19) 0.00976(19) 0.0051(3) 0.000 0.000 0.00488(9)
Rb2 0.01384(16) 0.01384(16) 0.0188(2) 0.000 0.000 0.00692(8)
O1 0.0162(7) 0.0148(7) 0.0120(6) -0.0003(6) 0.0063(6) 0.0079(6)
C1 0.0138(10) 0.0138(10) 0.0218(13) -0.0049(7) 0.0049(7) 0.0040(11)

_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
Co1 Rb2 4.17711(18) 1_565 ?
Co1 Rb2 4.17711(19) 1_455 ?
Co1 Rb2 4.17711(19) . ?
Co1 O1 2.1043(12) 3_655 ?
Co1 O1 2.1043(12) 5_665 ?
Co1 O1 2.1043(12) 11_655 ?
Co1 O1 2.1043(12) 10_665 ?
Co1 O1 2.1043(12) . ?
Co1 O1 2.1043(12) 12 ?
Rb2 Co1 4.17712(18) 1_545 ?
Rb2 Co1 4.17712(18) 1_655 ?
Rb2 Rb2 4.1463(2) 2_544 ?
Rb2 Rb2 4.1463(2) 2_545 ?
Rb2 O1 2.9443(13) 11_645 ?
Rb2 O1 2.9443(13) 12 ?
Rb2 O1 2.9443(13) 5_665 ?
Rb2 O1 2.9443(13) 3_755 ?
Rb2 O1 2.9443(13) 10_765 ?
Rb2 O1 2.9443(13) 1_545 ?
O1 Rb2 2.9443(13) 1_565 ?
O1 C1 1.2538(18) . ?
C1 O1 1.2538(18) 9_556 ?
C1 H1 0.9300 . ?

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
Rb2 Co1 Rb2 120.0 . 1_565 ?
Rb2 Co1 Rb2 120.0 1_565 1_455 ?
Rb2 Co1 Rb2 120.0 . 1_455 ?
O1 Co1 Rb2 41.30(3) 12 . ?
O1 Co1 Rb2 132.31(4) 11_655 1_455 ?
O1 Co1 Rb2 41.30(3) 5_665 . ?
O1 Co1 Rb2 132.31(4) 10_665 . ?
O1 Co1 Rb2 41.30(3) 10_665 1_455 ?
O1 Co1 Rb2 41.30(3) . 1_565 ?
O1 Co1 Rb2 94.48(4) 11_655 . ?
O1 Co1 Rb2 94.48(4) 12 1_455 ?
O1 Co1 Rb2 94.48(4) 3_655 . ?
O1 Co1 Rb2 132.31(4) 5_665 1_455 ?
O1 Co1 Rb2 132.31(4) 12 1_565 ?
O1 Co1 Rb2 41.30(3) 3_655 1_455 ?
O1 Co1 Rb2 94.48(4) 5_665 1_565 ?
O1 Co1 Rb2 94.48(4) . 1_455 ?
O1 Co1 Rb2 41.30(3) 11_655 1_565 ?
O1 Co1 Rb2 132.31(4) . . ?
O1 Co1 Rb2 94.48(4) 10_665 1_565 ?
O1 Co1 Rb2 132.31(4) 3_655 1_565 ?
O1 Co1 O1 91.36(5) 12 10_665 ?
O1 Co1 O1 95.38(7) 10_665 . ?
O1 Co1 O1 91.36(5) 5_665 3_655 ?
O1 Co1 O1 171.04(8) 5_665 10_665 ?
O1 Co1 O1 91.36(5) 12 11_655 ?
O1 Co1 O1 91.36(5) 11_655 10_665 ?
O1 Co1 O1 91.36(5) 3_655 . ?
O1 Co1 O1 82.60(7) 3_655 10_665 ?
O1 Co1 O1 82.60(7) 12 5_665 ?
O1 Co1 O1 171.04(8) 12 . ?
O1 Co1 O1 95.38(7) 12 3_655 ?
O1 Co1 O1 91.36(5) 5_665 . ?
O1 Co1 O1 171.04(8) 11_655 3_655 ?
O1 Co1 O1 82.60(7) 11_655 . ?
O1 Co1 O1 95.38(7) 5_665 11_655 ?
Co1 Rb2 Co1 120.0 1_655 1_545 ?
Co1 Rb2 Co1 120.0 . 1_655 ?
Co1 Rb2 Co1 120.0 . 1_545 ?
Rb2 Rb2 Co1 90.0 2_545 1_545 ?
Rb2 Rb2 Co1 90.0 2_545 . ?
Rb2 Rb2 Co1 90.0 2_544 . ?
Rb2 Rb2 Co1 90.0 2_544 1_545 ?
Rb2 Rb2 Co1 90.0 2_545 1_655 ?
Rb2 Rb2 Co1 90.0 2_544 1_655 ?
Rb2 Rb2 Rb2 180.0 2_545 2_544 ?
O1 Rb2 Co1 130.81(3) 11_645 . ?
O1 Rb2 Co1 130.81(3) 5_665 1_545 ?
O1 Rb2 Co1 103.19(3) 3_755 1_545 ?
O1 Rb2 Co1 130.81(3) 3_755 . ?
O1 Rb2 Co1 103.19(3) 5_665 1_655 ?
O1 Rb2 Co1 103.19(3) 10_765 . ?
O1 Rb2 Co1 28.14(2) 1_545 1_545 ?
O1 Rb2 Co1 103.19(3) 1_545 . ?
O1 Rb2 Co1 130.81(3) 1_545 1_655 ?
O1 Rb2 Co1 28.14(2) 12 . ?
O1 Rb2 Co1 28.14(2) 11_645 1_545 ?
O1 Rb2 Co1 28.14(2) 5_665 . ?
O1 Rb2 Co1 130.81(3) 10_765 1_545 ?
O1 Rb2 Co1 103.19(3) 11_645 1_655 ?
O1 Rb2 Co1 103.19(3) 12 1_545 ?
O1 Rb2 Co1 28.14(2) 3_755 1_655 ?
O1 Rb2 Co1 28.14(2) 10_765 1_655 ?
O1 Rb2 Co1 130.81(3) 12 1_655 ?
O1 Rb2 Rb2 66.25(2) 11_645 2_544 ?
O1 Rb2 Rb2 66.25(2) 10_765 2_544 ?
O1 Rb2 Rb2 113.75(2) 12 2_545 ?
O1 Rb2 Rb2 66.25(2) 3_755 2_545 ?
O1 Rb2 Rb2 66.25(2) 5_665 2_545 ?
O1 Rb2 Rb2 113.75(2) 10_765 2_545 ?
O1 Rb2 Rb2 113.75(2) 11_645 2_545 ?
O1 Rb2 Rb2 66.25(2) 1_545 2_545 ?
O1 Rb2 Rb2 113.75(2) 1_545 2_544 ?
O1 Rb2 Rb2 66.25(2) 12 2_544 ?
O1 Rb2 Rb2 113.75(2) 5_665 2_544 ?
O1 Rb2 Rb2 113.75(2) 3_755 2_544 ?
O1 Rb2 O1 104.87(3) 10_765 12 ?
O1 Rb2 O1 104.87(3) 11_645 10_765 ?
O1 Rb2 O1 153.61(5) 10_765 1_545 ?
O1 Rb2 O1 98.39(5) 1_545 12 ?
O1 Rb2 O1 56.29(5) 11_645 1_545 ?
O1 Rb2 O1 153.61(5) 11_645 5_665 ?
O1 Rb2 O1 98.39(5) 11_645 3_755 ?
O1 Rb2 O1 104.87(3) 3_755 5_665 ?
O1 Rb2 O1 153.61(5) 3_755 12 ?
O1 Rb2 O1 98.39(5) 10_765 5_665 ?
O1 Rb2 O1 104.87(3) 3_755 1_545 ?
O1 Rb2 O1 104.87(3) 1_545 5_665 ?
O1 Rb2 O1 104.87(3) 11_645 12 ?
O1 Rb2 O1 56.29(5) 12 5_665 ?
O1 Rb2 O1 56.29(5) 3_755 10_765 ?
Co1 O1 Rb2 110.56(5) . 1_565 ?
C1 O1 Co1 122.63(15) . . ?
C1 O1 Rb2 124.79(12) . 1_565 ?
O1 C1 O1 125.2(3) . 9_556 ?
O1 C1 H1 117.4 . . ?
O1 C1 H1 117.4 9_556 . ?

_shelx_res_file                  
;
    15smb009.res created by SHELXL-2014/7

TITL 15SMB009 in P6322 #182
REM reset to P6322 #182
CELL 0.71073 7.234961 7.234961 8.292577 90 90 120
ZERR 2 0.000322 0.000322 0.000404 0 0 0
LATT -1
SYMM -Y+X,+X,0.5+Z
SYMM -Y,+X-Y,+Z
SYMM -X,-Y,0.5+Z
SYMM +Y-X,-X,+Z
SYMM +Y,-X+Y,0.5+Z
SYMM -Y+X,-Y,-Z
SYMM -X,-X+Y,-Z
SYMM +Y,+X,-Z
SYMM -Y,-X,0.5-Z
SYMM +Y-X,+Y,0.5-Z
SYMM +X,+X-Y,0.5-Z
SFAC C H O Co Rb
UNIT 6 6 12 2 2

L.S. 4 0 0
PLAN  20
BOND
MORE -1
BOND $H
CONF
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\15SMB009.hkl">
REM </olex2.extras>

WGHT    0.015600    0.010300
FVAR       6.57732
CO1   4    0.666667    0.333333    0.250000    10.16667    0.00976    0.00976 =
         0.00510    0.00000    0.00000    0.00488
RB2   5    1.000000    0.000000    0.250000    10.16667    0.01384    0.01384 =
         0.01881    0.00000    0.00000    0.00692
O1    3    0.692902    0.585645    0.392999    11.00000    0.01618    0.01477 =
         0.01196   -0.00026    0.00626    0.00787
C1    1    0.559520    0.559520    0.500000    10.50000    0.01377    0.01377 =
         0.02181   -0.00494    0.00494    0.00401
AFIX  43
H1    2    0.430978    0.430978    0.499999    10.50000   -1.20000
AFIX   0
HKLF 4

REM  15SMB009 in P6322 #182
REM R1 =  0.0151 for     323 Fo > 4sig(Fo)  and  0.0166 for all     336 data
REM     19 parameters refined using      0 restraints

END

WGHT      0.0156      0.0103

REM Highest difference peak  0.237,  deepest hole -0.458,  1-sigma level  0.071
Q1    1   0.3333  0.6667  0.3830  10.33333  0.05    0.24
Q2    1   1.0767  0.0767  0.0000  10.50000  0.05    0.22
Q3    1   0.6667  0.3333  0.5061  10.33333  0.05    0.20
Q4    1   0.8994  0.8199  0.4423  11.00000  0.05    0.19
Q5    1   0.8464 -0.1584  0.3654  11.00000  0.05    0.18
Q6    1   0.8046 -0.0961  0.0672  11.00000  0.05    0.18
Q7    1   0.5650  0.2949  0.5748  11.00000  0.05    0.17
Q8    1   0.6174  0.4013  0.5096  11.00000  0.05    0.17
Q9    1   0.6628  0.6068  0.2438  11.00000  0.05    0.17
Q10   1   0.6684  0.5973  0.4531  11.00000  0.05    0.17
Q11   1   0.6471  0.8238  0.2920  11.00000  0.05    0.16
Q12   1   0.5725  0.7862  0.2500  10.50000  0.05    0.16
Q13   1   0.8009  0.7059  0.2404  11.00000  0.05    0.15
Q14   1   0.1430  0.1430  0.5000  10.50000  0.05    0.15
Q15   1   0.7583  0.5169  0.4917  11.00000  0.05    0.15
Q16   1   0.7193  0.4155  0.4085  11.00000  0.05    0.15
Q17   1   0.8469 -0.1473  0.1251  11.00000  0.05    0.14
Q18   1   0.9456 -0.1084  0.1212  11.00000  0.05    0.14
Q19   1   0.7579  0.5829  0.3170  11.00000  0.05    0.14
Q20   1   0.5898  0.4386  0.4073  11.00000  0.05    0.13
;
_shelx_res_checksum              85999
_shelx_SHELXL_version_number     2014/7
_olex2_date_sample_data_collection 2015-02-18
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_Compound3
_database_code_depnum_ccdc_archive 'CCDC 1417124'
_audit_update_record             
;
2015-08-05 deposited with the CCDC.
2016-03-24 downloaded from the CCDC.
;

_audit_creation_date             2012-01-16T17:07:26-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C3 H3 Ni O6 Rb'
_chemical_formula_sum            'C3 H3 Ni O6 Rb'
_chemical_formula_weight         279.23
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Rb Ni C3 O6'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rb Rb -0.4688 1.6079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           182
_space_group_name_H-M_alt        'P 63 2 2'
_space_group_name_Hall           'P 6c 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'

_cell_length_a                   7.2095(3)
_cell_length_b                   7.2095(3)
_cell_length_c                   8.1492(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     366.83(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1554
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      75.6420
_cell_measurement_theta_min      7.0730
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    11.807
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81039
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    2.528
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             268
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_unetI/netI     0.0110
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2630
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.693
_diffrn_reflns_theta_min         7.093
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector_area_resol_mean 10.5035
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   -6.00   33.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.5000   30.0000   60.0000 39

#__ type_ start__ end____ width___ exp.time_
  2 omega  -82.00  -24.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.5000  -37.0000 -180.0000 58

#__ type_ start__ end____ width___ exp.time_
  3 omega -110.00  -15.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.5000  -77.0000    0.0000 95

#__ type_ start__ end____ width___ exp.time_
  4 omega  -43.00   34.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.5000   30.0000  -30.0000 77

#__ type_ start__ end____ width___ exp.time_
  5 omega   61.00   87.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       42.4552 -125.0000  177.0000 26

#__ type_ start__ end____ width___ exp.time_
  6 omega    8.00   57.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       42.4552  -99.0000  150.0000 49

#__ type_ start__ end____ width___ exp.time_
  7 omega   42.00   69.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -150.0000 27

#__ type_ start__ end____ width___ exp.time_
  8 omega   45.00   84.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  -90.0000 39

#__ type_ start__ end____ width___ exp.time_
  9 omega   31.00   68.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -90.0000 37

#__ type_ start__ end____ width___ exp.time_
 10 omega  137.00  175.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   15.0000  -30.0000 38

#__ type_ start__ end____ width___ exp.time_
 11 omega   58.00  119.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   60.0000 61

#__ type_ start__ end____ width___ exp.time_
 12 omega  106.00  172.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000 -120.0000 66

#__ type_ start__ end____ width___ exp.time_
 13 omega   43.00   86.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  150.0000 43

#__ type_ start__ end____ width___ exp.time_
 14 omega   73.00  120.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -150.0000 47

#__ type_ start__ end____ width___ exp.time_
 15 omega   43.00   94.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000    0.0000 51

#__ type_ start__ end____ width___ exp.time_
 16 omega  135.00  161.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000  -90.0000 26

#__ type_ start__ end____ width___ exp.time_
 17 omega   41.00   86.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000  -60.0000 45

#__ type_ start__ end____ width___ exp.time_
 18 omega   41.00   87.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  120.0000 46

#__ type_ start__ end____ width___ exp.time_
 19 omega   41.00  100.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000  -90.0000 59

#__ type_ start__ end____ width___ exp.time_
 20 omega   81.00  121.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   15.0000  -30.0000 40

#__ type_ start__ end____ width___ exp.time_
 21 omega   84.00  109.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -90.0000 25

#__ type_ start__ end____ width___ exp.time_
 22 omega   74.00  106.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -120.0000 32

#__ type_ start__ end____ width___ exp.time_
 23 omega   99.00  147.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -15.0000   60.0000 48

#__ type_ start__ end____ width___ exp.time_
 24 omega   32.00   70.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -15.0000   60.0000 38
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.1396578000
_diffrn_orient_matrix_UB_12      0.0233063000
_diffrn_orient_matrix_UB_13      -0.1503172000
_diffrn_orient_matrix_UB_21      0.1708312000
_diffrn_orient_matrix_UB_22      0.0003517000
_diffrn_orient_matrix_UB_23      0.1138917000
_diffrn_orient_matrix_UB_31      -0.1102569000
_diffrn_orient_matrix_UB_32      -0.2455251000
_diffrn_orient_matrix_UB_33      -0.0141649000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.406
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                258
_reflns_number_total             263
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 
;
 Flack x determined using 75 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.001(19)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     19
_refine_ls_number_reflns         263
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0135
_refine_ls_R_factor_gt           0.0130
_refine_ls_restrained_S_all      1.183
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0210P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0321
_refine_ls_wR_factor_ref         0.0322
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   ?
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
Ni1 Ni 0.6667 0.3333 0.2500 0.00945(18) Uani 1 6 d S T P . .
Rb2 Rb 1.0000 0.0000 0.2500 0.01696(15) Uani 1 6 d S T P . .
O1 O 0.4180(2) 0.3088(2) 0.10735(16) 0.0149(3) Uani 1 1 d . . . . .
C1 C 0.4445(4) 0.4445(4) 0.0000 0.0164(5) Uani 1 2 d S T P . .
H1 H 0.5735 0.5735 0.0000 0.020 Uiso 1 2 calc RS T P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.0109(2) 0.0109(2) 0.0065(3) 0.000 0.000 0.00545(12)
Rb2 0.01538(17) 0.01538(17) 0.0201(2) 0.000 0.000 0.00769(9)
O1 0.0146(6) 0.0175(6) 0.0126(6) 0.0058(5) 0.0000(5) 0.0080(5)
C1 0.0133(8) 0.0133(8) 0.0178(13) 0.0047(5) -0.0047(5) 0.0031(10)

_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
Ni1 Rb2 4.16242(19) 1_455 ?
Ni1 Rb2 4.16242(18) 1_565 ?
Ni1 Rb2 4.16242(19) . ?
Ni1 O1 2.0683(12) 5_665 ?
Ni1 O1 2.0683(12) 11_655 ?
Ni1 O1 2.0683(12) 10_665 ?
Ni1 O1 2.0683(12) 12 ?
Ni1 O1 2.0683(12) . ?
Ni1 O1 2.0683(12) 3_655 ?
Rb2 Ni1 4.16243(19) 1_545 ?
Rb2 Ni1 4.16243(19) 1_655 ?
Rb2 Rb2 4.0746(2) 2_544 ?
Rb2 Rb2 4.0746(2) 2_545 ?
Rb2 O1 2.9464(13) 12_655 ?
Rb2 O1 2.9464(13) 10_655 ?
Rb2 O1 2.9464(13) 11_655 ?
Rb2 O1 2.9464(13) 1_655 ?
Rb2 O1 2.9464(13) 5_655 ?
Rb2 O1 2.9464(13) 3_655 ?
O1 Rb2 2.9464(13) 1_455 ?
O1 C1 1.2542(18) . ?
C1 O1 1.2542(18) 9 ?
C1 H1 0.9300 . ?

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
Rb2 Ni1 Rb2 120.0 . 1_455 ?
Rb2 Ni1 Rb2 120.0 1_455 1_565 ?
Rb2 Ni1 Rb2 120.0 . 1_565 ?
O1 Ni1 Rb2 132.56(4) 11_655 1_455 ?
O1 Ni1 Rb2 94.25(4) 5_665 . ?
O1 Ni1 Rb2 132.56(4) . . ?
O1 Ni1 Rb2 94.25(4) 3_655 1_455 ?
O1 Ni1 Rb2 132.56(4) 3_655 1_565 ?
O1 Ni1 Rb2 94.25(4) 12 . ?
O1 Ni1 Rb2 94.25(4) 11_655 1_565 ?
O1 Ni1 Rb2 41.37(3) 3_655 . ?
O1 Ni1 Rb2 94.25(4) . 1_565 ?
O1 Ni1 Rb2 132.56(4) 10_665 . ?
O1 Ni1 Rb2 41.37(3) 5_665 1_565 ?
O1 Ni1 Rb2 41.37(3) 10_665 1_565 ?
O1 Ni1 Rb2 41.37(3) 11_655 . ?
O1 Ni1 Rb2 132.56(4) 5_665 1_455 ?
O1 Ni1 Rb2 94.25(4) 10_665 1_455 ?
O1 Ni1 Rb2 41.37(3) 12 1_455 ?
O1 Ni1 Rb2 132.56(4) 12 1_565 ?
O1 Ni1 Rb2 41.37(3) . 1_455 ?
O1 Ni1 O1 91.50(5) 11_655 10_665 ?
O1 Ni1 O1 171.49(7) 11_655 . ?
O1 Ni1 O1 91.50(5) 5_665 . ?
O1 Ni1 O1 82.73(7) 11_655 3_655 ?
O1 Ni1 O1 91.50(5) 12 10_665 ?
O1 Ni1 O1 82.73(7) 12 . ?
O1 Ni1 O1 171.49(7) 3_655 10_665 ?
O1 Ni1 O1 94.89(7) 10_665 . ?
O1 Ni1 O1 91.50(5) 11_655 12 ?
O1 Ni1 O1 91.50(5) 3_655 . ?
O1 Ni1 O1 94.89(7) 3_655 12 ?
O1 Ni1 O1 91.50(5) 3_655 5_665 ?
O1 Ni1 O1 94.89(7) 11_655 5_665 ?
O1 Ni1 O1 82.73(7) 5_665 10_665 ?
O1 Ni1 O1 171.49(7) 12 5_665 ?
Ni1 Rb2 Ni1 120.0 1_655 1_545 ?
Ni1 Rb2 Ni1 120.0 . 1_655 ?
Ni1 Rb2 Ni1 120.0 . 1_545 ?
Rb2 Rb2 Ni1 90.0 2_545 1_655 ?
Rb2 Rb2 Ni1 90.0 2_544 1_655 ?
Rb2 Rb2 Ni1 90.0 2_545 . ?
Rb2 Rb2 Ni1 90.0 2_545 1_545 ?
Rb2 Rb2 Ni1 90.0 2_544 1_545 ?
Rb2 Rb2 Ni1 90.0 2_544 . ?
Rb2 Rb2 Rb2 180.0 2_545 2_544 ?
O1 Rb2 Ni1 130.87(3) 12_655 . ?
O1 Rb2 Ni1 103.39(2) 10_655 . ?
O1 Rb2 Ni1 103.39(2) 11_655 1_655 ?
O1 Rb2 Ni1 103.39(2) 3_655 1_545 ?
O1 Rb2 Ni1 27.64(2) 1_655 1_655 ?
O1 Rb2 Ni1 130.87(3) 5_655 . ?
O1 Rb2 Ni1 103.39(2) 12_655 1_545 ?
O1 Rb2 Ni1 27.64(2) 5_655 1_545 ?
O1 Rb2 Ni1 27.64(2) 10_655 1_545 ?
O1 Rb2 Ni1 103.39(2) 5_655 1_655 ?
O1 Rb2 Ni1 130.87(3) 11_655 1_545 ?
O1 Rb2 Ni1 27.64(2) 3_655 . ?
O1 Rb2 Ni1 130.87(3) 10_655 1_655 ?
O1 Rb2 Ni1 27.64(2) 11_655 . ?
O1 Rb2 Ni1 130.87(3) 3_655 1_655 ?
O1 Rb2 Ni1 27.64(2) 12_655 1_655 ?
O1 Rb2 Ni1 130.87(3) 1_655 1_545 ?
O1 Rb2 Ni1 103.39(2) 1_655 . ?
O1 Rb2 Rb2 113.24(3) 12_655 2_544 ?
O1 Rb2 Rb2 113.24(3) 11_655 2_544 ?
O1 Rb2 Rb2 113.24(3) 1_655 2_545 ?
O1 Rb2 Rb2 66.76(3) 1_655 2_544 ?
O1 Rb2 Rb2 66.76(3) 10_655 2_545 ?
O1 Rb2 Rb2 66.76(3) 12_655 2_545 ?
O1 Rb2 Rb2 113.24(3) 5_655 2_545 ?
O1 Rb2 Rb2 113.24(3) 10_655 2_544 ?
O1 Rb2 Rb2 113.24(3) 3_655 2_545 ?
O1 Rb2 Rb2 66.76(3) 3_655 2_544 ?
O1 Rb2 Rb2 66.76(3) 11_655 2_545 ?
O1 Rb2 Rb2 66.76(3) 5_655 2_544 ?
O1 Rb2 O1 105.46(3) 10_655 11_655 ?
O1 Rb2 O1 153.22(5) 12_655 3_655 ?
O1 Rb2 O1 98.27(5) 1_655 11_655 ?
O1 Rb2 O1 98.27(5) 10_655 3_655 ?
O1 Rb2 O1 98.27(5) 12_655 5_655 ?
O1 Rb2 O1 105.46(3) 5_655 3_655 ?
O1 Rb2 O1 105.46(3) 5_655 1_655 ?
O1 Rb2 O1 105.46(3) 12_655 10_655 ?
O1 Rb2 O1 105.46(3) 12_655 11_655 ?
O1 Rb2 O1 153.22(5) 10_655 1_655 ?
O1 Rb2 O1 55.28(5) 5_655 10_655 ?
O1 Rb2 O1 153.22(5) 5_655 11_655 ?
O1 Rb2 O1 55.28(5) 12_655 1_655 ?
O1 Rb2 O1 55.28(5) 11_655 3_655 ?
O1 Rb2 O1 105.46(3) 1_655 3_655 ?
Ni1 O1 Rb2 110.99(5) . 1_455 ?
C1 O1 Ni1 122.55(14) . . ?
C1 O1 Rb2 124.32(12) . 1_455 ?
O1 C1 O1 124.4(2) . 9 ?
O1 C1 H1 117.8 . . ?
O1 C1 H1 117.8 9 . ?

_shelx_res_file                  
;
    15smb025.res created by SHELXL-2014/7

TITL 15smb025 in P6322 #182
REM reset to P6322 #182
CELL 1.54184 7.209515 7.209515 8.149244 90 90 120
ZERR 2 0.000331 0.000331 0.00042 0 0 0
LATT -1
SYMM -Y+X,+X,0.5+Z
SYMM -Y,+X-Y,+Z
SYMM -X,-Y,0.5+Z
SYMM +Y-X,-X,+Z
SYMM +Y,-X+Y,0.5+Z
SYMM -Y+X,-Y,-Z
SYMM -X,-X+Y,-Z
SYMM +Y,+X,-Z
SYMM -Y,-X,0.5-Z
SYMM +Y-X,+Y,0.5-Z
SYMM +X,+X-Y,0.5-Z
SFAC C H O Ni Rb
UNIT 6 6 12 2 2

L.S. 4
PLAN  20
BOND
MORE -1
BOND $H
CONF
fmap 2
ACTA
REM <olex2.extras>
REM <HklSrc "%.\\15smb025.hkl">
REM </olex2.extras>

WGHT    0.021000
FVAR       0.96063
NI1   4    0.666667    0.333333    0.250000    10.16667    0.01090    0.01090 =
         0.00653    0.00000    0.00000    0.00545
RB2   5    1.000000    0.000000    0.250000    10.16667    0.01538    0.01538 =
         0.02011    0.00000    0.00000    0.00769
O1    3    0.418048    0.308758    0.107349    11.00000    0.01457    0.01752 =
         0.01263    0.00582   -0.00002    0.00797
C1    1    0.444523    0.444523    0.000000    10.50000    0.01328    0.01328 =
         0.01782    0.00469   -0.00469    0.00313
AFIX  43
H1    2    0.573520    0.573520    0.000002    10.50000   -1.20000
AFIX   0
HKLF 4

REM  15smb025 in P6322 #182
REM R1 =  0.0130 for     258 Fo > 4sig(Fo)  and  0.0135 for all     263 data
REM     19 parameters refined using      0 restraints

END

WGHT      0.0210      0.0000

REM Highest difference peak  0.318,  deepest hole -0.350,  1-sigma level  0.070
Q1    1   1.0000  0.0000  0.0000  10.16667  0.05    0.32
Q2    1   0.3333  0.6667  0.1101  10.33333  0.05    0.17
Q3    1   0.6667  0.3333  0.1069  10.33333  0.05    0.16
Q4    1   0.6667  0.3333 -0.0087  10.33333  0.05    0.14
Q5    1   0.1799  0.3404  0.1794  11.00000  0.05    0.12
Q6    1   0.8255  0.8338  0.0629  11.00000  0.05    0.12
Q7    1   0.2742  0.2713  0.1706  11.00000  0.05    0.11
Q8    1   0.2439  0.4879  0.2500  10.50000  0.05    0.11
Q9    1   0.2679  0.3705  0.1728  11.00000  0.05    0.10
Q10   1   0.3995  0.3192  0.2868  11.00000  0.05    0.10
Q11   1   0.3627  0.4343  0.1761  11.00000  0.05    0.10
Q12   1   0.5055  0.6584  0.0587  11.00000  0.05    0.09
Q13   1   0.2730  0.1535  0.0817  11.00000  0.05    0.09
Q14   1   1.0782 -0.1156  0.0721  11.00000  0.05    0.08
Q15   1   0.3113  0.4593  0.2298  11.00000  0.05    0.08
Q16   1   0.2937  0.2857  0.2833  11.00000  0.05    0.08
Q17   1   0.6449  0.5643  0.0892  11.00000  0.05    0.08
Q18   1   0.5468  0.2234  0.0499  11.00000  0.05    0.06
Q19   1   0.3701  0.4225  0.2704  11.00000  0.05    0.06
Q20   1   0.7211  0.7211  0.0000  10.50000  0.05    0.04
;
_shelx_res_checksum              61145
_shelx_SHELXL_version_number     2014/7
_olex2_date_sample_data_collection 2015-05-22
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_Compound4
_database_code_depnum_ccdc_archive 'CCDC 1417125'
_audit_update_record             
;
2015-08-05 deposited with the CCDC.
2016-03-24 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT987_Compound4           
;
PROBLEM: The Flack x is &gt;&gt; 0 -  Do a BASF/TWIN Refinement     Please Check
RESPONSE: A twin refinement has been completed and details included in the CIF indicating the presence of a merohedral racemic twin
;
_vrf_STRVA01_Compound4           
;
PROBLEM: Flack test results are ambiguous.
RESPONSE: A twin refinement has been completed and details included in the CIF indicating the presence of a merohedral racemic twin
;

# Added during the CSD deposition process: Wednesday 5th of August 2015 06:12:49 PM
# end Validation Reply Form


_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C3 H3 Cs Mn O6'
_chemical_formula_sum            'C3 H3 Cs Mn O6'
_chemical_formula_weight         322.90
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           182
_space_group_name_H-M_alt        'P 63 2 2'
_space_group_name_Hall           'P 6c 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'

_cell_length_a                   7.58190(10)
_cell_length_b                   7.58190(10)
_cell_length_c                   8.3786(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     417.117(15)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    346
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  1.0
_exptl_absorpt_correction_T_max  1.2118
_exptl_crystal_colour            'translucent colourless'
_exptl_crystal_density_diffrn    2.571
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       'hexagonal block'
_exptl_crystal_F_000             298
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.200
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.046
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_number            9467
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.446
_diffrn_reflns_theta_min         4.866
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_reflns_Friedel_coverage         0.440
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                218
_reflns_number_total             225
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         1.184
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.56(11)
_refine_ls_extinction_coef       0.072(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.362
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     21
_refine_ls_number_reflns         225
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0196
_refine_ls_R_factor_gt           0.0189
_refine_ls_restrained_S_all      1.362
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0177P)²+0.0901P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0490
_refine_ls_wR_factor_ref         0.0492
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.44(11) 0.56(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Mn1 Mn -0.3333 -0.6667 -0.7500 0.0108(3) Uani 1 6 d S T P . .
Cs2 Cs 0.0000 -1.0000 -0.7500 0.0182(3) Uani 1 6 d S T P . .
O1 O -0.5817(3) -0.6925(3) -0.8990(3) 0.0183(5) Uani 1 1 d . . . . .
C1 C -0.5610(8) -0.5610(8) -1.0000 0.0195(10) Uani 1 2 d S T P . .
H1 H -0.4384 -0.4384 -1.0000 0.023 Uiso 1 2 calc RS T P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mn1 0.0116(4) 0.0116(4) 0.0091(5) 0.000 0.000 0.00579(19)
Cs2 0.0157(3) 0.0157(3) 0.0233(3) 0.000 0.000 0.00785(14)
O1 0.0163(12) 0.0204(13) 0.0176(10) 0.0069(11) -0.0011(10) 0.0088(10)
C1 0.0149(15) 0.0149(15) 0.024(2) 0.0069(11) -0.0069(11) 0.0041(19)

_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
Mn1 Cs2 4.37741(5) 1_565 ?
Mn1 Cs2 4.37741(5) 1_455 ?
Mn1 Cs2 4.37741(6) . ?
Mn1 O1 2.185(2) 12_543 ?
Mn1 O1 2.185(2) 3_445 ?
Mn1 O1 2.185(2) 5_545 ?
Mn1 O1 2.185(2) 10_443 ?
Mn1 O1 2.185(2) . ?
Mn1 O1 2.185(2) 11_553 ?
Cs2 Mn1 4.37743(5) 1_545 ?
Cs2 Mn1 4.37742(6) 1_655 ?
Cs2 Cs2 4.18930(9) 2_445 ?
Cs2 Cs2 4.18930(9) 2_444 ?
Cs2 O1 3.108(2) 12_643 ?
Cs2 O1 3.108(2) 3_445 ?
Cs2 O1 3.108(2) 1_655 ?
Cs2 O1 3.108(2) 5_535 ?
Cs2 O1 3.108(2) 10_433 ?
Cs2 O1 3.108(2) 11_553 ?
O1 Cs2 3.108(2) 1_455 ?
O1 C1 1.256(3) . ?
C1 O1 1.256(3) 9_553 ?
C1 H1 0.9300 . ?

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
Cs2 Mn1 Cs2 120.0 . 1_565 ?
Cs2 Mn1 Cs2 120.0 1_565 1_455 ?
Cs2 Mn1 Cs2 120.0 . 1_455 ?
O1 Mn1 Cs2 41.73(6) 11_553 . ?
O1 Mn1 Cs2 131.98(6) 5_545 1_455 ?
O1 Mn1 Cs2 41.73(6) 3_445 . ?
O1 Mn1 Cs2 131.98(6) 10_443 . ?
O1 Mn1 Cs2 94.45(6) 10_443 1_455 ?
O1 Mn1 Cs2 94.45(6) . 1_565 ?
O1 Mn1 Cs2 94.45(6) 5_545 . ?
O1 Mn1 Cs2 131.98(6) 11_553 1_455 ?
O1 Mn1 Cs2 94.45(6) 12_543 . ?
O1 Mn1 Cs2 94.45(6) 3_445 1_455 ?
O1 Mn1 Cs2 94.45(6) 11_553 1_565 ?
O1 Mn1 Cs2 41.73(6) 12_543 1_455 ?
O1 Mn1 Cs2 131.98(6) 3_445 1_565 ?
O1 Mn1 Cs2 41.73(6) . 1_455 ?
O1 Mn1 Cs2 41.73(6) 5_545 1_565 ?
O1 Mn1 Cs2 131.98(6) . . ?
O1 Mn1 Cs2 41.73(6) 10_443 1_565 ?
O1 Mn1 Cs2 131.98(6) 12_543 1_565 ?
O1 Mn1 O1 90.59(8) 11_553 10_443 ?
O1 Mn1 O1 96.05(12) 10_443 . ?
O1 Mn1 O1 96.05(12) 3_445 12_543 ?
O1 Mn1 O1 171.11(12) 3_445 10_443 ?
O1 Mn1 O1 96.05(12) 11_553 5_545 ?
O1 Mn1 O1 83.45(11) 5_545 10_443 ?
O1 Mn1 O1 83.45(11) 12_543 . ?
O1 Mn1 O1 90.59(8) 12_543 10_443 ?
O1 Mn1 O1 83.45(11) 11_553 3_445 ?
O1 Mn1 O1 171.11(12) 11_553 . ?
O1 Mn1 O1 90.59(8) 11_553 12_543 ?
O1 Mn1 O1 90.59(8) 3_445 . ?
O1 Mn1 O1 171.11(12) 5_545 12_543 ?
O1 Mn1 O1 90.59(8) 5_545 . ?
O1 Mn1 O1 90.59(8) 3_445 5_545 ?
Mn1 Cs2 Mn1 120.0 1_655 1_545 ?
Mn1 Cs2 Mn1 120.0 . 1_655 ?
Mn1 Cs2 Mn1 120.0 . 1_545 ?
Cs2 Cs2 Mn1 90.0 2_444 1_545 ?
Cs2 Cs2 Mn1 90.0 2_444 . ?
Cs2 Cs2 Mn1 90.0 2_445 . ?
Cs2 Cs2 Mn1 90.0 2_445 1_545 ?
Cs2 Cs2 Mn1 90.0 2_444 1_655 ?
Cs2 Cs2 Mn1 90.0 2_445 1_655 ?
Cs2 Cs2 Cs2 180.0 2_444 2_445 ?
O1 Cs2 Mn1 130.52(4) 12_643 . ?
O1 Cs2 Mn1 130.52(4) 1_655 1_545 ?
O1 Cs2 Mn1 27.90(4) 5_535 1_545 ?
O1 Cs2 Mn1 130.52(4) 5_535 . ?
O1 Cs2 Mn1 27.90(4) 1_655 1_655 ?
O1 Cs2 Mn1 103.53(4) 10_433 . ?
O1 Cs2 Mn1 130.52(4) 11_553 1_545 ?
O1 Cs2 Mn1 27.90(4) 11_553 . ?
O1 Cs2 Mn1 103.53(4) 11_553 1_655 ?
O1 Cs2 Mn1 27.90(4) 3_445 . ?
O1 Cs2 Mn1 103.53(4) 12_643 1_545 ?
O1 Cs2 Mn1 103.53(4) 1_655 . ?
O1 Cs2 Mn1 27.90(4) 10_433 1_545 ?
O1 Cs2 Mn1 27.90(4) 12_643 1_655 ?
O1 Cs2 Mn1 103.53(4) 3_445 1_545 ?
O1 Cs2 Mn1 103.53(4) 5_535 1_655 ?
O1 Cs2 Mn1 130.52(4) 10_433 1_655 ?
O1 Cs2 Mn1 130.52(4) 3_445 1_655 ?
O1 Cs2 Cs2 66.31(4) 12_643 2_445 ?
O1 Cs2 Cs2 66.31(4) 10_433 2_445 ?
O1 Cs2 Cs2 66.31(4) 3_445 2_444 ?
O1 Cs2 Cs2 66.31(4) 5_535 2_444 ?
O1 Cs2 Cs2 66.31(4) 1_655 2_444 ?
O1 Cs2 Cs2 113.69(4) 10_433 2_444 ?
O1 Cs2 Cs2 113.69(4) 12_643 2_444 ?
O1 Cs2 Cs2 113.69(4) 11_553 2_444 ?
O1 Cs2 Cs2 66.31(4) 11_553 2_445 ?
O1 Cs2 Cs2 113.69(4) 3_445 2_445 ?
O1 Cs2 Cs2 113.69(4) 1_655 2_445 ?
O1 Cs2 Cs2 113.69(4) 5_535 2_445 ?
O1 Cs2 O1 98.95(9) 10_433 3_445 ?
O1 Cs2 O1 104.95(5) 12_643 10_433 ?
O1 Cs2 O1 104.95(5) 10_433 11_553 ?
O1 Cs2 O1 55.81(8) 11_553 3_445 ?
O1 Cs2 O1 104.95(5) 12_643 11_553 ?
O1 Cs2 O1 55.81(8) 12_643 1_655 ?
O1 Cs2 O1 98.95(8) 12_643 5_535 ?
O1 Cs2 O1 104.95(5) 5_535 1_655 ?
O1 Cs2 O1 104.95(5) 5_535 3_445 ?
O1 Cs2 O1 152.94(8) 10_433 1_655 ?
O1 Cs2 O1 152.94(8) 5_535 11_553 ?
O1 Cs2 O1 98.95(9) 11_553 1_655 ?
O1 Cs2 O1 152.94(8) 12_643 3_445 ?
O1 Cs2 O1 104.95(5) 3_445 1_655 ?
O1 Cs2 O1 55.81(8) 5_535 10_433 ?
Mn1 O1 Cs2 110.37(8) . 1_455 ?
C1 O1 Mn1 123.6(3) . . ?
C1 O1 Cs2 122.8(2) . 1_455 ?
O1 C1 O1 125.3(5) . 9_553 ?
O1 C1 H1 117.3 . . ?
O1 C1 H1 117.3 9_553 . ?

_shelx_res_file                  
;
    shelx.res created by SHELXL-2014/7

TITL shelx in P6322 #182
REM reset to P6322 #182
CELL 0.71073 7.5819 7.5819 8.3786 90 90 120
ZERR 2 0.0001 0.0001 0.0002 0 0 0
LATT -1
SYMM -Y+X,+X,0.5+Z
SYMM -Y,+X-Y,+Z
SYMM -X,-Y,0.5+Z
SYMM +Y-X,-X,+Z
SYMM +Y,-X+Y,0.5+Z
SYMM -Y+X,-Y,-Z
SYMM -X,-X+Y,-Z
SYMM +Y,+X,-Z
SYMM -Y,-X,0.5-Z
SYMM +Y-X,+Y,0.5-Z
SYMM +X,+X-Y,0.5-Z
SFAC Mn C H O Cs
UNIT 2 6 6 12 2

L.S. 10
PLAN  25
BOND
MORE -1
BOND $H
CONF
fmap 2
acta
TWIN -1 0 0 0 -1 0 0 0 -1 2
OMIT 0 1 0
OMIT 0 1 1
REM <olex2.extras>
REM <HklSrc "%.\\shelx.hkl">
REM </olex2.extras>

WGHT    0.017700    0.090100
EXTI    0.072383
BASF   0.55826
FVAR       0.53837
MN1   1   -0.333333   -0.666667   -0.750000    10.16667    0.01159    0.01159 =
         0.00914    0.00000    0.00000    0.00579
CS2   5    0.000000   -1.000000   -0.750000    10.16667    0.01570    0.01570 =
         0.02332    0.00000    0.00000    0.00785
O1    4   -0.581723   -0.692463   -0.899016    11.00000    0.01634    0.02038 =
         0.01763    0.00694   -0.00108    0.00885
C1    2   -0.561014   -0.561014   -1.000000    10.50000    0.01489    0.01489 =
         0.02424    0.00692   -0.00692    0.00411
AFIX  43
H1    3   -0.438353   -0.438353   -0.999999    10.50000   -1.20000
AFIX   0
HKLF 4

REM  shelx in P6322 #182
REM R1 =  0.0189 for     218 Fo > 4sig(Fo)  and  0.0196 for all     225 data
REM     21 parameters refined using      0 restraints

END

WGHT      0.0177      0.0901

REM Highest difference peak  1.184,  deepest hole -0.669,  1-sigma level  0.122
Q1    1  -0.6667 -0.3333 -0.7500  10.16667  0.05    1.18
Q2    1  -0.6641 -0.8460 -1.0016  11.00000  0.05    0.24
Q3    1  -0.3290 -0.4205 -0.9075  11.00000  0.05    0.23
Q4    1  -0.4218 -0.6135 -0.8622  11.00000  0.05    0.22
Q5    1  -0.8015 -0.7749 -0.9302  11.00000  0.05    0.20
Q6    1  -0.4064 -0.3029 -0.9033  11.00000  0.05    0.18
Q7    1  -0.7186 -0.8611 -0.8898  11.00000  0.05    0.18
Q8    1   0.0055 -1.1041 -0.8794  11.00000  0.05    0.17
Q9    1  -0.6859 -0.5945 -0.9023  11.00000  0.05    0.17
Q10   1  -0.2010 -0.1767 -0.9370  11.00000  0.05    0.16
Q11   1   0.0000 -1.0000 -0.8988  10.33333  0.05    0.16
Q12   1  -0.7368 -0.7368 -1.0000  10.50000  0.05    0.16
Q13   1  -0.7422 -0.9572 -0.8939  11.00000  0.05    0.16
Q14   1  -0.0877 -1.0739 -0.8900  11.00000  0.05    0.15
Q15   1  -0.8392 -0.7205 -0.9028  11.00000  0.05    0.14
Q16   1  -0.3333 -0.6667 -1.0433  10.33333  0.05    0.14
Q17   1  -0.6667 -0.3333 -0.8754  10.33333  0.05    0.14
Q18   1  -0.3588 -0.6407 -0.9313  11.00000  0.05    0.14
Q19   1   0.0000 -1.1027 -1.0000  10.50000  0.05    0.13
Q20   1  -0.5962 -0.7785 -0.8043  11.00000  0.05    0.12
Q21   1  -0.6614 -0.8307 -0.7500  10.50000  0.05    0.12
Q22   1  -0.5931 -0.6492 -0.7516  11.00000  0.05    0.12
Q23   1  -0.6531 -0.6055 -0.7541  11.00000  0.05    0.11
Q24   1   0.1277 -1.0000 -1.0000  10.50000  0.05    0.11
Q25   1  -0.8165 -0.6330 -0.7500  10.50000  0.05    0.10
;
_shelx_res_checksum              54879
_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.44(11)
2 0.56(11)
####################################################################### 
# 
# 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_Compound5
_database_code_depnum_ccdc_archive 'CCDC 1417126'
_audit_update_record             
;
2015-08-05 deposited with the CCDC.
2016-03-24 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT430_Compound5           
;
PROBLEM: Short Inter D...A Contact  O1     ..  O1      ..       2.22 Ang.
RESPONSE: There are no hydrogen atoms missing in the structure - the atoms are both in the same formate ligand
;

# Added during the CSD deposition process: Wednesday 5th of August 2015 06:12:49 PM
# end Validation Reply Form


_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C3 H3 Co Cs O6'
_chemical_formula_sum            'C3 H3 Co Cs O6'
_chemical_formula_weight         326.89
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Cs Co C3 O6 H3'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           182
_space_group_name_H-M_alt        'P 63 2 2'
_space_group_name_Hall           'P 6c 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'

_cell_length_a                   7.5112(3)
_cell_length_b                   7.5112(3)
_cell_length_c                   8.0670(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     394.15(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2247
_cell_measurement_temperature    150.0(3)
_cell_measurement_theta_max      29.3160
_cell_measurement_theta_min      4.0070
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    6.709
_exptl_absorpt_correction_T_max  0.688
_exptl_absorpt_correction_T_min  0.527
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.754
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       'hexagonal block'
_exptl_crystal_F_000             302
_exptl_crystal_size_max          0.1434
_exptl_crystal_size_mid          0.1128
_exptl_crystal_size_min          0.0694
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_unetI/netI     0.0154
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3248
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.421
_diffrn_reflns_theta_min         3.132
_diffrn_ambient_temperature      150.0(3)
_diffrn_detector_area_resol_mean 10.4102
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -14.00   26.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -10.0516  -99.0000 -180.0000 40

#__ type_ start__ end____ width___ exp.time_
  2 omega   -5.00   85.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4813   38.0000 -150.0000 90

#__ type_ start__ end____ width___ exp.time_
  3 omega   20.00   81.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4813 -147.0000   34.0000 61

#__ type_ start__ end____ width___ exp.time_
  4 omega  -63.00   32.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4813  -57.0000   60.0000 95
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0366983000
_diffrn_orient_matrix_UB_12      0.0565262000
_diffrn_orient_matrix_UB_13      -0.0446688000
_diffrn_orient_matrix_UB_21      -0.0121940000
_diffrn_orient_matrix_UB_22      0.0413061000
_diffrn_orient_matrix_UB_23      0.0754228000
_diffrn_orient_matrix_UB_31      0.1019547000
_diffrn_orient_matrix_UB_32      0.0835469000
_diffrn_orient_matrix_UB_33      -0.0070649000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.429
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.940
_reflns_number_gt                340
_reflns_number_total             363
_reflns_odcompleteness_completeness 99.50
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.360
_refine_diff_density_min         -1.237
_refine_diff_density_rms         0.147
_refine_ls_abs_structure_details 
;
 Flack x determined using 97 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.000(18)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     19
_refine_ls_number_reflns         363
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0189
_refine_ls_R_factor_gt           0.0167
_refine_ls_restrained_S_all      1.163
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0211P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0372
_refine_ls_wR_factor_ref         0.0378
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   ?
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
Co1 Co 1.6667 1.3333 1.2500 0.00744(18) Uani 1 6 d S T P . .
Cs1 Cs 2.0000 1.0000 1.2500 0.01440(14) Uani 1 6 d S T P . .
O1 O 1.8856(3) 1.5743(3) 1.1023(2) 0.0129(4) Uani 1 1 d . . . . .
C1 C 2.0000 1.5543(6) 1.0000 0.0140(8) Uani 1 2 d S T P . .
H1 H 2.0000 1.4305 1.0000 0.017 Uiso 1 2 calc RS T P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0081(2) 0.0081(2) 0.0060(3) 0.000 0.000 0.00407(12)
Cs1 0.01304(16) 0.01304(16) 0.0171(2) 0.000 0.000 0.00652(8)
O1 0.0132(9) 0.0124(9) 0.0120(8) 0.0003(8) 0.0053(8) 0.0055(7)
C1 0.016(2) 0.0105(11) 0.017(2) 0.0039(8) 0.0078(17) 0.0082(10)

_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
Co1 Cs1 4.33658(17) 1_455 ?
Co1 Cs1 4.33658(17) 1_565 ?
Co1 Cs1 4.33658(18) . ?
Co1 O1 2.1033(18) 10_887 ?
Co1 O1 2.1033(18) . ?
Co1 O1 2.1033(17) 5_785 ?
Co1 O1 2.1033(17) 11_757 ?
Co1 O1 2.1033(17) 3_865 ?
Co1 O1 2.1033(17) 12_567 ?
Cs1 O1 3.1037(18) 10_987 ?
Cs1 O1 3.1037(18) 5_785 ?
Cs1 O1 3.1037(18) 3_965 ?
Cs1 O1 3.1037(18) 1_545 ?
Cs1 O1 3.1037(18) 11_747 ?
Cs1 O1 3.1037(17) 12_567 ?
Cs1 C1 3.908(4) 5_785 ?
Cs1 C1 3.908(4) 6_565 ?
Cs1 C1 3.908(4) 1_545 ?
Cs1 C1 3.908(4) 4_985 ?
Cs1 C1 3.908(4) 2_745 ?
Cs1 C1 3.908(4) 3_965 ?
O1 Cs1 3.1037(17) 1_565 ?
O1 C1 1.254(3) . ?
C1 Cs1 3.908(4) 2_654 ?
C1 Cs1 3.908(4) 1_565 ?
C1 O1 1.254(3) 8_977 ?
C1 H1 0.9300 . ?

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
Cs1 Co1 Cs1 120.0 . 1_455 ?
Cs1 Co1 Cs1 120.0 1_455 1_565 ?
Cs1 Co1 Cs1 120.0 . 1_565 ?
O1 Co1 Cs1 41.81(5) 5_785 . ?
O1 Co1 Cs1 41.81(5) . 1_565 ?
O1 Co1 Cs1 41.81(5) 12_567 . ?
O1 Co1 Cs1 132.63(5) 11_757 . ?
O1 Co1 Cs1 41.81(5) 11_757 1_565 ?
O1 Co1 Cs1 41.81(5) 3_865 1_455 ?
O1 Co1 Cs1 93.90(5) . . ?
O1 Co1 Cs1 132.63(5) 5_785 1_565 ?
O1 Co1 Cs1 93.90(5) 10_887 . ?
O1 Co1 Cs1 93.90(5) 12_567 1_565 ?
O1 Co1 Cs1 93.90(5) 5_785 1_455 ?
O1 Co1 Cs1 132.63(5) 10_887 1_565 ?
O1 Co1 Cs1 132.63(5) 12_567 1_455 ?
O1 Co1 Cs1 93.90(5) 3_865 1_565 ?
O1 Co1 Cs1 132.63(5) . 1_455 ?
O1 Co1 Cs1 132.63(5) 3_865 . ?
O1 Co1 Cs1 93.90(5) 11_757 1_455 ?
O1 Co1 Cs1 41.81(5) 10_887 1_455 ?
O1 Co1 O1 172.19(10) 5_785 11_757 ?
O1 Co1 O1 94.74(10) 11_757 3_865 ?
O1 Co1 O1 94.74(11) 5_785 10_887 ?
O1 Co1 O1 91.08(7) 12_567 11_757 ?
O1 Co1 O1 91.08(7) 5_785 . ?
O1 Co1 O1 83.62(10) . 11_757 ?
O1 Co1 O1 83.62(10) 10_887 3_865 ?
O1 Co1 O1 91.08(7) 10_887 11_757 ?
O1 Co1 O1 83.62(10) 5_785 12_567 ?
O1 Co1 O1 91.08(7) 5_785 3_865 ?
O1 Co1 O1 94.74(11) 12_567 . ?
O1 Co1 O1 172.19(10) 12_567 3_865 ?
O1 Co1 O1 172.19(10) . 10_887 ?
O1 Co1 O1 91.08(7) . 3_865 ?
O1 Co1 O1 91.08(7) 12_567 10_887 ?
O1 Cs1 O1 98.54(7) 10_987 1_545 ?
O1 Cs1 O1 98.54(7) 3_965 12_567 ?
O1 Cs1 O1 106.20(4) 3_965 5_785 ?
O1 Cs1 O1 106.20(4) 10_987 11_747 ?
O1 Cs1 O1 106.20(4) 1_545 5_785 ?
O1 Cs1 O1 53.72(7) 1_545 11_747 ?
O1 Cs1 O1 106.20(4) 11_747 12_567 ?
O1 Cs1 O1 53.72(7) 10_987 3_965 ?
O1 Cs1 O1 152.27(7) 10_987 5_785 ?
O1 Cs1 O1 106.20(4) 1_545 3_965 ?
O1 Cs1 O1 98.54(7) 11_747 5_785 ?
O1 Cs1 O1 152.27(6) 11_747 3_965 ?
O1 Cs1 O1 53.72(7) 12_567 5_785 ?
O1 Cs1 O1 152.27(7) 1_545 12_567 ?
O1 Cs1 O1 106.20(4) 10_987 12_567 ?
O1 Cs1 C1 164.14(4) 10_987 5_785 ?
O1 Cs1 C1 15.86(4) 3_965 3_965 ?
O1 Cs1 C1 68.80(4) 1_545 6_565 ?
O1 Cs1 C1 90.35(4) 1_545 5_785 ?
O1 Cs1 C1 90.35(4) 3_965 1_545 ?
O1 Cs1 C1 89.65(4) 11_747 5_785 ?
O1 Cs1 C1 89.65(4) 5_785 6_565 ?
O1 Cs1 C1 111.20(4) 3_965 5_785 ?
O1 Cs1 C1 15.86(4) 1_545 1_545 ?
O1 Cs1 C1 68.80(4) 12_567 5_785 ?
O1 Cs1 C1 111.20(4) 5_785 1_545 ?
O1 Cs1 C1 15.86(4) 5_785 5_785 ?
O1 Cs1 C1 164.14(4) 3_965 6_565 ?
O1 Cs1 C1 164.14(4) 1_545 4_985 ?
O1 Cs1 C1 111.20(4) 1_545 3_965 ?
O1 Cs1 C1 111.20(4) 11_747 4_985 ?
O1 Cs1 C1 90.35(4) 5_785 3_965 ?
O1 Cs1 C1 89.65(4) 3_965 4_985 ?
O1 Cs1 C1 68.80(4) 11_747 1_545 ?
O1 Cs1 C1 15.86(4) 12_567 4_985 ?
O1 Cs1 C1 164.14(4) 12_567 1_545 ?
O1 Cs1 C1 68.80(4) 5_785 4_985 ?
O1 Cs1 C1 111.20(4) 10_987 6_565 ?
O1 Cs1 C1 15.86(4) 10_987 2_745 ?
O1 Cs1 C1 15.86(4) 11_747 6_565 ?
O1 Cs1 C1 89.65(4) 1_545 2_745 ?
O1 Cs1 C1 90.35(4) 12_567 6_565 ?
O1 Cs1 C1 90.35(4) 11_747 2_745 ?
O1 Cs1 C1 68.80(4) 10_987 3_965 ?
O1 Cs1 C1 68.80(4) 3_965 2_745 ?
O1 Cs1 C1 164.14(4) 11_747 3_965 ?
O1 Cs1 C1 111.20(4) 12_567 2_745 ?
O1 Cs1 C1 89.65(4) 12_567 3_965 ?
O1 Cs1 C1 164.14(4) 5_785 2_745 ?
O1 Cs1 C1 89.65(4) 10_987 1_545 ?
O1 Cs1 C1 90.35(4) 10_987 4_985 ?
C1 Cs1 C1 84.23(4) 5_785 6_565 ?
C1 Cs1 C1 95.77(4) 5_785 1_545 ?
C1 Cs1 C1 180.0 4_985 1_545 ?
C1 Cs1 C1 95.77(4) 4_985 6_565 ?
C1 Cs1 C1 84.23(4) 4_985 3_965 ?
C1 Cs1 C1 95.77(4) 2_745 6_565 ?
C1 Cs1 C1 84.23(4) 5_785 4_985 ?
C1 Cs1 C1 84.23(4) 1_545 6_565 ?
C1 Cs1 C1 95.77(4) 5_785 3_965 ?
C1 Cs1 C1 84.23(4) 2_745 1_545 ?
C1 Cs1 C1 84.23(4) 2_745 3_965 ?
C1 Cs1 C1 180.0 5_785 2_745 ?
C1 Cs1 C1 180.00(11) 6_565 3_965 ?
C1 Cs1 C1 95.77(4) 4_985 2_745 ?
C1 Cs1 C1 95.77(4) 1_545 3_965 ?
Co1 O1 Cs1 111.33(7) . 1_565 ?
C1 O1 Co1 123.9(2) . . ?
C1 O1 Cs1 121.55(18) . 1_565 ?
Cs1 C1 Cs1 62.13(6) 1_565 2_654 ?
Cs1 C1 H1 148.9 2_654 . ?
Cs1 C1 H1 148.9 1_565 . ?
O1 C1 Cs1 42.59(15) 8_977 2_654 ?
O1 C1 Cs1 42.59(16) . 1_565 ?
O1 C1 Cs1 86.8(2) 8_977 1_565 ?
O1 C1 Cs1 86.8(2) . 2_654 ?
O1 C1 O1 124.9(4) . 8_977 ?
O1 C1 H1 117.6 . . ?
O1 C1 H1 117.6 8_977 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Co1 O1 C1 Cs1 151.17(13) . . . 2_654 ?
Co1 O1 C1 Cs1 -157.9(2) . . . 1_565 ?
Co1 O1 C1 O1 171.41(17) . . . 8_977 ?
Cs1 O1 C1 Cs1 -50.93(10) 1_565 . . 2_654 ?
Cs1 O1 C1 O1 -30.69(8) 1_565 . . 8_977 ?

_shelx_res_file                  
;
    015smb013.res created by SHELXL-2014/7

TITL 015SMB013 in P6322 #182
REM reset to P6322 #182
CELL 0.71073 7.511183 7.511183 8.066977 90 90 120
ZERR 2 0.000289 0.000289 0.000388 0 0 0
LATT -1
SYMM -Y+X,+X,0.5+Z
SYMM -Y,+X-Y,+Z
SYMM -X,-Y,0.5+Z
SYMM +Y-X,-X,+Z
SYMM +Y,-X+Y,0.5+Z
SYMM -Y+X,-Y,-Z
SYMM -X,-X+Y,-Z
SYMM +Y,+X,-Z
SYMM -Y,-X,0.5-Z
SYMM +Y-X,+Y,0.5-Z
SYMM +X,+X-Y,0.5-Z
SFAC Cs Co C O H
UNIT 2 2 6 12 6

L.S. 10
PLAN  20
BOND
MORE -1
BOND $H
CONF
fmap 2
acta 52
REM <olex2.extras>
REM <HklSrc "%.\\015SMB013.hkl">
REM </olex2.extras>

WGHT    0.021100
FVAR       0.73919
CO1   2    1.666667    1.333333    1.250000    10.16667    0.00814    0.00814 =
         0.00603    0.00000    0.00000    0.00407
CS1   1    2.000000    1.000000    1.250000    10.16667    0.01304    0.01304 =
         0.01713    0.00000    0.00000    0.00652
O1    4    1.885648    1.574331    1.102336    11.00000    0.01315    0.01240 =
         0.01197    0.00028    0.00527    0.00552
C1    3    2.000000    1.554279    1.000000    10.50000    0.01633    0.01046 =
         0.01706    0.00391    0.00783    0.00817
AFIX  43
H1    5    2.000001    1.430465    1.000000    10.50000   -1.20000
AFIX   0
HKLF 4

REM  015SMB013 in P6322 #182
REM R1 =  0.0167 for     340 Fo > 4sig(Fo)  and  0.0189 for all     363 data
REM     19 parameters refined using      0 restraints

END

WGHT      0.0211      0.0000

REM Highest difference peak  0.360,  deepest hole -1.237,  1-sigma level  0.147
Q1    1   1.9803  1.4853  1.1865  11.00000  0.05    0.36
Q2    1   1.6667  1.3333  0.9710  10.33333  0.05    0.35
Q3    1   2.0446  1.6657  1.1676  11.00000  0.05    0.27
Q4    1   1.9236  1.6281  1.1588  11.00000  0.05    0.27
Q5    1   2.1124  1.5514  1.1520  11.00000  0.05    0.26
Q6    1   1.8387  1.6805  1.1930  11.00000  0.05    0.26
Q7    1   2.0948  1.1784  1.1688  11.00000  0.05    0.25
Q8    1   1.7203  1.4434  0.9975  11.00000  0.05    0.25
Q9    1   1.6667  1.3333  1.0878  10.33333  0.05    0.24
Q10   1   1.8279  1.4823  1.1363  11.00000  0.05    0.23
Q11   1   2.1108  1.0000  1.0000  10.50000  0.05    0.23
Q12   1   2.2116  1.7802  1.1608  11.00000  0.05    0.22
Q13   1   2.0023  1.7318  1.2452  11.00000  0.05    0.21
Q14   1   1.9439  1.7035  1.1611  11.00000  0.05    0.21
Q15   1   1.7939  1.4777  1.0384  11.00000  0.05    0.20
Q16   1   1.7565  1.4917  0.9237  11.00000  0.05    0.20
Q17   1   1.9360  1.5788  1.2493  11.00000  0.05    0.20
Q18   1   2.1508  1.8533  1.1512  11.00000  0.05    0.20
Q19   1   1.7644  1.3947  1.0537  11.00000  0.05    0.19
Q20   1   2.2385  1.6147  1.1143  11.00000  0.05    0.18
;
_shelx_res_checksum              56118
_shelx_SHELXL_version_number     2014/7
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1 8 -4 0.0612 0.9960 7.9938 -3.9938 0.5937 0.0168 0.7976
10 -1 2 0.0514 9.9891 -0.9982 2.0024 -0.5125 -0.0120 0.9209
-7 9 -5 0.0488 -6.9952 8.9922 -4.9962 0.9882 0.0799 0.0734
5 -6 -9 0.0326 4.9931 -5.9946 -8.9910 -0.1205 -0.9866 0.0718
-7 4 8 0.0323 -6.9907 3.9960 7.9905 0.1255 0.8530 -0.4353
-6 -5 -1 0.0749 -5.9922 -4.9966 -1.0030 -0.0177 -0.2090 -1.0213
8 -3 -8 0.0574 7.9893 -2.9967 -7.9898 -0.1057 -0.8238 0.6206
-4 6 9 0.0358 -3.9943 5.9947 8.9915 0.0838 0.9745 0.0301
-1 -8 3 0.0723 -0.9963 -7.9938 2.9948 -0.5491 -0.0922 -0.7906
8 -9 5 0.0471 7.9940 -8.9921 4.9967 -1.0249 -0.0920 0.0285
-10 1 -2 0.0675 -9.9891 0.9982 -2.0024 0.5125 0.0120 -0.9209

_olex2_date_sample_data_collection 2015-03-05
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_Compound6
_database_code_depnum_ccdc_archive 'CCDC 1417127'
_audit_update_record             
;
2015-08-05 deposited with the CCDC.
2016-03-24 downloaded from the CCDC.
;

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C3 H3 Cs Ni O6'
_chemical_formula_sum            'C3 H3 Cs Ni O6'
_chemical_formula_weight         326.67
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           182
_space_group_name_H-M_alt        'P 63 2 2'
_space_group_name_Hall           'P 6c 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'

_cell_length_a                   7.4866(7)
_cell_length_b                   7.4866(7)
_cell_length_c                   7.8898(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     382.97(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1517
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      29.6330
_cell_measurement_theta_min      4.0730
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    7.197
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72675
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    2.833
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             304
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3112
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.773
_diffrn_reflns_theta_min         4.068
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector_area_resol_mean 10.5035
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -19.00   47.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        9.9525  -99.0000   30.0000 66

#__ type_ start__ end____ width___ exp.time_
  2 omega  -17.00   80.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        9.9525   57.0000 -150.0000 97

#__ type_ start__ end____ width___ exp.time_
  3 omega  -61.00   18.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        9.9525  -37.0000   60.0000 79

#__ type_ start__ end____ width___ exp.time_
  4 omega  -32.00   12.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -10.3431  -77.0000 -120.0000 44
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0940446000
_diffrn_orient_matrix_UB_12      0.0014452000
_diffrn_orient_matrix_UB_13      0.0012230000
_diffrn_orient_matrix_UB_21      0.0486069000
_diffrn_orient_matrix_UB_22      0.0938124000
_diffrn_orient_matrix_UB_23      0.0462055000
_diffrn_orient_matrix_UB_31      0.0275957000
_diffrn_orient_matrix_UB_32      0.0561400000
_diffrn_orient_matrix_UB_33      -0.0771228000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.414
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.888
_reflns_number_gt                325
_reflns_number_total             352
_reflns_odcompleteness_completeness 98.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.648
_refine_diff_density_min         -1.153
_refine_diff_density_rms         0.165
_refine_ls_abs_structure_details 
;
 Flack x determined using 94 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     19
_refine_ls_number_reflns         352
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0265
_refine_ls_restrained_S_all      1.154
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0401P)²+0.4005P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0693
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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
Cs1 Cs 0.0000 0.0000 0.2500 0.0203(3) Uani 1 6 d S T P . .
Ni2 Ni 0.3333 0.6667 0.7500 0.0072(3) Uani 1 6 d S T P . .
O2 O 0.3128(5) 0.8836(5) 0.6025(4) 0.0128(6) Uani 1 1 d . . . . .
C1 C 0.4490(9) 1.0000 0.5000 0.0134(13) Uani 1 2 d S T P . .
H1 H 0.5733 1.0000 0.5000 0.016 Uiso 1 2 calc RS T P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cs1 0.0161(3) 0.0161(3) 0.0287(4) 0.000 0.000 0.00803(15)
Ni2 0.0077(4) 0.0077(4) 0.0062(5) 0.000 0.000 0.00386(19)
O2 0.0147(16) 0.0142(16) 0.0117(14) 0.0063(13) 0.0037(14) 0.0088(15)
C1 0.009(2) 0.014(3) 0.019(3) 0.009(3) 0.0044(13) 0.0070(16)

_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
Cs1 O2 3.105(3) 7_666 ?
Cs1 O2 3.105(3) 9_456 ?
Cs1 O2 3.105(3) 2_654 ?
Cs1 O2 3.105(3) 6_444 ?
Cs1 O2 3.105(3) 8_546 ?
Cs1 O2 3.105(3) 4_564 ?
Cs1 C1 3.898(6) 6_444 ?
Cs1 C1 3.898(6) 2_654 ?
Cs1 C1 3.898(6) 5_455 ?
Cs1 C1 3.898(6) 3_665 ?
Cs1 C1 3.898(6) 1_545 ?
Cs1 C1 3.898(6) 4_564 ?
Ni2 Cs1 4.3224(4) 2_565 ?
Ni2 Cs1 4.3224(4) 2 ?
Ni2 Cs1 4.3224(4) 2_665 ?
Ni2 O2 2.065(3) 3_665 ?
Ni2 O2 2.065(3) 11_556 ?
Ni2 O2 2.065(3) . ?
Ni2 O2 2.065(3) 12_566 ?
Ni2 O2 2.065(3) 5_565 ?
Ni2 O2 2.065(3) 10_666 ?
O2 Cs1 3.105(3) 2_565 ?
O2 C1 1.251(4) . ?
C1 Cs1 3.898(6) 2_565 ?
C1 Cs1 3.898(6) 1_565 ?
C1 O2 1.251(4) 7_676 ?
C1 H1 0.9300 . ?

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 Cs1 O2 98.43(13) 7_666 6_444 ?
O2 Cs1 O2 106.81(6) 8_546 9_456 ?
O2 Cs1 O2 98.43(13) 8_546 4_564 ?
O2 Cs1 O2 106.81(6) 7_666 8_546 ?
O2 Cs1 O2 151.85(12) 7_666 4_564 ?
O2 Cs1 O2 52.63(11) 6_444 8_546 ?
O2 Cs1 O2 151.85(12) 6_444 9_456 ?
O2 Cs1 O2 52.63(11) 7_666 2_654 ?
O2 Cs1 O2 98.43(13) 2_654 9_456 ?
O2 Cs1 O2 106.81(6) 6_444 2_654 ?
O2 Cs1 O2 106.81(6) 6_444 4_564 ?
O2 Cs1 O2 151.85(12) 8_546 2_654 ?
O2 Cs1 O2 106.81(6) 2_654 4_564 ?
O2 Cs1 O2 106.81(6) 7_666 9_456 ?
O2 Cs1 O2 52.63(11) 9_456 4_564 ?
O2 Cs1 C1 89.17(7) 2_654 3_665 ?
O2 Cs1 C1 112.20(6) 6_444 2_654 ?
O2 Cs1 C1 90.83(7) 7_666 3_665 ?
O2 Cs1 C1 67.80(6) 4_564 3_665 ?
O2 Cs1 C1 67.80(6) 9_456 4_564 ?
O2 Cs1 C1 89.17(7) 6_444 1_545 ?
O2 Cs1 C1 112.20(6) 8_546 3_665 ?
O2 Cs1 C1 67.80(6) 2_654 1_545 ?
O2 Cs1 C1 89.17(7) 9_456 2_654 ?
O2 Cs1 C1 164.01(6) 4_564 1_545 ?
O2 Cs1 C1 15.99(6) 4_564 4_564 ?
O2 Cs1 C1 67.80(6) 6_444 5_455 ?
O2 Cs1 C1 164.01(6) 6_444 3_665 ?
O2 Cs1 C1 164.01(6) 2_654 5_455 ?
O2 Cs1 C1 89.17(7) 4_564 5_455 ?
O2 Cs1 C1 15.99(6) 9_456 3_665 ?
O2 Cs1 C1 89.17(7) 7_666 6_444 ?
O2 Cs1 C1 15.99(6) 7_666 1_545 ?
O2 Cs1 C1 15.99(6) 6_444 6_444 ?
O2 Cs1 C1 90.83(7) 8_546 1_545 ?
O2 Cs1 C1 67.80(6) 8_546 6_444 ?
O2 Cs1 C1 112.20(6) 9_456 1_545 ?
O2 Cs1 C1 90.83(7) 2_654 6_444 ?
O2 Cs1 C1 112.20(6) 7_666 5_455 ?
O2 Cs1 C1 164.01(6) 9_456 6_444 ?
O2 Cs1 C1 15.99(6) 8_546 5_455 ?
O2 Cs1 C1 112.20(6) 4_564 6_444 ?
O2 Cs1 C1 90.83(7) 9_456 5_455 ?
O2 Cs1 C1 164.01(6) 7_666 4_564 ?
O2 Cs1 C1 67.80(6) 7_666 2_654 ?
O2 Cs1 C1 90.83(7) 6_444 4_564 ?
O2 Cs1 C1 15.99(6) 2_654 2_654 ?
O2 Cs1 C1 89.17(7) 8_546 4_564 ?
O2 Cs1 C1 90.83(7) 4_564 2_654 ?
O2 Cs1 C1 112.20(6) 2_654 4_564 ?
O2 Cs1 C1 164.01(6) 8_546 2_654 ?
C1 Cs1 C1 83.35(7) 6_444 5_455 ?
C1 Cs1 C1 96.65(7) 6_444 2_654 ?
C1 Cs1 C1 180.0 5_455 2_654 ?
C1 Cs1 C1 83.35(7) 4_564 5_455 ?
C1 Cs1 C1 83.35(7) 3_665 2_654 ?
C1 Cs1 C1 96.65(7) 3_665 5_455 ?
C1 Cs1 C1 83.35(7) 6_444 1_545 ?
C1 Cs1 C1 96.65(7) 1_545 5_455 ?
C1 Cs1 C1 96.65(7) 4_564 2_654 ?
C1 Cs1 C1 96.65(7) 6_444 4_564 ?
C1 Cs1 C1 83.35(7) 1_545 2_654 ?
C1 Cs1 C1 180.0 6_444 3_665 ?
C1 Cs1 C1 96.65(7) 3_665 1_545 ?
C1 Cs1 C1 83.35(7) 4_564 3_665 ?
C1 Cs1 C1 180.0 4_564 1_545 ?
Cs1 Ni2 Cs1 120.0 2_665 2 ?
Cs1 Ni2 Cs1 120.0 2_565 2_665 ?
Cs1 Ni2 Cs1 120.0 2_565 2 ?
O2 Ni2 Cs1 132.92(10) 12_566 2_565 ?
O2 Ni2 Cs1 93.69(10) 5_565 2 ?
O2 Ni2 Cs1 41.81(9) 3_665 2 ?
O2 Ni2 Cs1 132.92(10) 5_565 2_565 ?
O2 Ni2 Cs1 93.69(10) 10_666 2 ?
O2 Ni2 Cs1 93.69(10) . 2_665 ?
O2 Ni2 Cs1 41.81(9) . 2_565 ?
O2 Ni2 Cs1 132.92(10) 10_666 2_665 ?
O2 Ni2 Cs1 132.92(10) . 2 ?
O2 Ni2 Cs1 41.81(9) 11_556 2_665 ?
O2 Ni2 Cs1 132.92(10) 11_556 2 ?
O2 Ni2 Cs1 132.92(10) 3_665 2_665 ?
O2 Ni2 Cs1 41.81(9) 12_566 2 ?
O2 Ni2 Cs1 93.69(10) 12_566 2_665 ?
O2 Ni2 Cs1 41.81(9) 5_565 2_665 ?
O2 Ni2 Cs1 93.69(10) 11_556 2_565 ?
O2 Ni2 Cs1 93.69(10) 3_665 2_565 ?
O2 Ni2 Cs1 41.81(9) 10_666 2_565 ?
O2 Ni2 O2 172.62(19) 11_556 3_665 ?
O2 Ni2 O2 91.35(12) 3_665 5_565 ?
O2 Ni2 O2 94.16(19) 10_666 3_665 ?
O2 Ni2 O2 172.62(19) . 12_566 ?
O2 Ni2 O2 83.61(17) . 10_666 ?
O2 Ni2 O2 91.35(12) 10_666 12_566 ?
O2 Ni2 O2 83.61(18) 11_556 5_565 ?
O2 Ni2 O2 91.35(12) 11_556 12_566 ?
O2 Ni2 O2 94.16(19) 12_566 5_565 ?
O2 Ni2 O2 83.61(18) 3_665 12_566 ?
O2 Ni2 O2 94.16(19) . 11_556 ?
O2 Ni2 O2 91.35(12) . 5_565 ?
O2 Ni2 O2 91.35(12) . 3_665 ?
O2 Ni2 O2 172.62(19) 10_666 5_565 ?
O2 Ni2 O2 91.35(12) 10_666 11_556 ?
Ni2 O2 Cs1 111.88(12) . 2_565 ?
C1 O2 Cs1 120.9(3) . 2_565 ?
C1 O2 Ni2 123.9(4) . . ?
Cs1 C1 Cs1 60.80(10) 1_565 2_565 ?
Cs1 C1 H1 149.6 2_565 . ?
Cs1 C1 H1 149.6 1_565 . ?
O2 C1 Cs1 43.1(3) . 2_565 ?
O2 C1 Cs1 43.1(3) 7_676 1_565 ?
O2 C1 Cs1 85.7(3) . 1_565 ?
O2 C1 Cs1 85.7(3) 7_676 2_565 ?
O2 C1 O2 124.4(6) 7_676 . ?
O2 C1 H1 117.8 7_676 . ?
O2 C1 H1 117.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cs1 O2 C1 Cs1 -50.60(17) 2_565 . . 1_565 ?
Cs1 O2 C1 O2 -30.34(14) 2_565 . . 7_676 ?
Ni2 O2 C1 Cs1 -157.5(4) . . . 2_565 ?
Ni2 O2 C1 Cs1 151.9(2) . . . 1_565 ?
Ni2 O2 C1 O2 172.2(3) . . . 7_676 ?

_shelx_res_file                  
;
    15smb021.res created by SHELXL-2014/7

TITL
CELL 0.71073 7.486599 7.486599 7.889821 90 90 120
ZERR 2 0.000691 0.000691 0.000832 0 0 0
LATT -1
SYMM -Y+X,+X,0.5+Z
SYMM -Y,+X-Y,+Z
SYMM -X,-Y,0.5+Z
SYMM +Y-X,-X,+Z
SYMM +Y,-X+Y,0.5+Z
SYMM -Y+X,-Y,-Z
SYMM -X,-X+Y,-Z
SYMM +Y,+X,-Z
SYMM -Y,-X,0.5-Z
SYMM +Y-X,+Y,0.5-Z
SYMM +X,+X-Y,0.5-Z
SFAC C H O Ni Cs
UNIT 6 6 12 2 2

L.S. 4
PLAN  20
MORE -1
BOND $H
CONF
fmap 2
acta 52
REM <olex2.extras>
REM <HklSrc "%.\\15SMB021.hkl">
REM </olex2.extras>

WGHT    0.040100    0.400500
FVAR       7.05227
CS1   5    0.000000    0.000000    0.250000    10.16667    0.01606    0.01606 =
         0.02866    0.00000    0.00000    0.00803
NI2   4    0.333333    0.666667    0.750000    10.16667    0.00773    0.00773 =
         0.00623    0.00000    0.00000    0.00386
O2    3    0.312824    0.883553    0.602495    11.00000    0.01475    0.01420 =
         0.01170    0.00629    0.00369    0.00884
C1    1    0.449035    1.000000    0.500000    10.50000    0.00868    0.01408 =
         0.01928    0.00877    0.00439    0.00704
AFIX  43
H1    2    0.573258    1.000002    0.500001    10.50000   -1.20000
AFIX   0
HKLF 4

REM
REM R1 =  0.0265 for     325 Fo > 4sig(Fo)  and  0.0296 for all     352 data
REM     19 parameters refined using      0 restraints

END

WGHT      0.0401      0.4005

REM Highest difference peak  1.648,  deepest hole -1.153,  1-sigma level  0.165
Q1    1   0.0000  0.0000  0.1346  10.33333  0.05    1.65
Q2    1   0.2997  0.8785  0.6871  11.00000  0.05    0.44
Q3    1   0.0000  0.0000  0.0000  10.16667  0.05    0.40
Q4    1   0.3498  0.8561  0.6438  11.00000  0.05    0.37
Q5    1   0.4797  1.1060  0.6298  11.00000  0.05    0.32
Q6    1   0.4850  1.2225  0.6865  11.00000  0.05    0.31
Q7    1   0.2412  0.7829  0.7033  11.00000  0.05    0.29
Q8    1   0.0684  0.7958  0.6538  11.00000  0.05    0.28
Q9    1   0.2089  0.9364  0.6496  11.00000  0.05    0.27
Q10   1   0.7745  1.0247  0.6398  11.00000  0.05    0.27
Q11   1   0.1783  1.0000  0.5000  10.50000  0.05    0.27
Q12   1   0.5207  0.8863  0.6418  11.00000  0.05    0.26
Q13   1   0.2892  0.7506  0.6106  11.00000  0.05    0.26
Q14   1   0.3384  1.0767  0.5621  11.00000  0.05    0.25
Q15   1   0.3379  0.8789  0.5224  11.00000  0.05    0.25
Q16   1   0.1617  0.9861  0.6002  11.00000  0.05    0.25
Q17   1   0.2564  0.8966  0.5607  11.00000  0.05    0.24
Q18   1   0.0837  0.8972  0.5012  11.00000  0.05    0.24
Q19   1   0.3336  0.9923  0.6267  11.00000  0.05    0.24
Q20   1   0.3882  1.1941  0.7500  10.50000  0.05    0.24
;
_shelx_res_checksum              33806
_shelx_SHELXL_version_number     2014/7
_olex2_date_sample_data_collection 2015-03-19
_olex2_submission_special_instructions 'No special instructions were received'

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
