Cages on a plane: a structural matrix for molecular 'sheets'.
Fraser, Hector W. L.; Nichol, Gary S.; Baldansuren, Amgalanbaatar; McInnes, Eric J. L.; Brechin, Euan K.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 15530–15537; doi:10.1039/c8dt03793k

data_7702241
_publ_section_title
;
 Cages on a plane: a structural matrix for molecular 'sheets'.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15530
_journal_page_last               15537
_journal_paper_doi               10.1039/c8dt03793k
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'C72 H72 Co5 Cr2 N12 O12, 4(Cl1 O4), 9 C H4 O'
_chemical_formula_sum            'C81 H108 Cl4 Co5 Cr2 N12 O37'
_chemical_formula_weight         2382.24
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-09-07
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_audit_update_record
;
2018-07-11 deposited with the CCDC.
2018-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   14.7268(2)
_cell_length_b                   14.7268(2)
_cell_length_c                   38.1319(8)
_cell_measurement_reflns_used    26180
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      28.9710
_cell_measurement_theta_min      3.1880
_cell_volume                     7162.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -88.00 -44.00   1.00   15.00    --   -9.43 162.00 167.05   44
  2  \w    -20.00  30.00   1.00   15.00    --   -9.43 -99.00  60.00   50
  3  \w    -46.00  69.00   1.00   15.00    --   -9.43  19.00-120.00  115
  4  \w    -41.00  64.00   1.00   15.00    --   -9.43  77.00  90.00  105
  5  \w    -20.00  15.00   1.00   15.00    --   -9.43 -99.00 150.00   35
  6  \w    -37.00 -10.00   1.00   15.00    --   -9.43  77.00 -60.00   27
  7  \w     16.00  42.00   1.00   15.00    --   -9.43  77.00 -60.00   26
  8  \w    -19.00  29.00   1.00   15.00    --   -9.43 -99.00-180.00   48
  9  \w    -20.00   5.00   1.00   15.00    --   -9.43 -99.00 -60.00   25
 10  \w    -30.00  -3.00   1.00   15.00    --   10.84 -38.00 150.00   27
 11  \w     25.00  50.00   1.00   15.00    --   10.84 -99.00-150.00   25
 12  \w     24.00  84.00   1.00   15.00    --   10.84-153.00  76.73   60
 13  \w     34.00  61.00   1.00   15.00    --   10.84-160.00 -67.34   27
 14  \w     -5.00  22.00   1.00   15.00    --   10.84-116.00-154.34   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0369109000
_diffrn_orient_matrix_UB_12      -0.0174025000
_diffrn_orient_matrix_UB_13      0.0014169000
_diffrn_orient_matrix_UB_21      -0.0063580000
_diffrn_orient_matrix_UB_22      -0.0128628000
_diffrn_orient_matrix_UB_23      -0.0180966000
_diffrn_orient_matrix_UB_31      0.0411202000
_diffrn_orient_matrix_UB_32      0.0512150000
_diffrn_orient_matrix_UB_33      -0.0040626000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            43856
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.648
_diffrn_reflns_theta_min         3.112
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.272
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9174
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0659 before and 0.0587 after correction.
The Ratio of minimum to maximum transmission is 0.9174.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark pink'
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_description       block
_exptl_crystal_F_000             3675
_exptl_crystal_recrystallization_method
'The material was recrystallised from methanol by hydrothermal bomb'
_exptl_crystal_size_max          0.322
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         4234
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0425
_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/[\s^2^(Fo^2^)+(0.0173P)^2^+27.2577P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.0914
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3674
_reflns_number_total             4234
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03793k2.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7702241
_chemical_oxdiff_formula         'C30 H30 N10 O10 Cr Cl Co'
_chemical_oxdiff_usercomment     '@ 120 K 698o'
_shelx_estimated_absorpt_t_max   0.883
_shelx_estimated_absorpt_t_min   0.685
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{Co1, Cr1}
3. Restrained distances
 Cl2-O5 \\sim Cl2-O6 \\sim Cl2-O6A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(Co1) = Uanis(Cr1)
5. Rigid body (RIGU) restrains
 Cl2, O5, O6, O6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O6A)=1-FVAR(1)
 Sof(O6)=FVAR(1)
 Fixed Sof: Co1(0.66666) Cr1(0.33333)
7.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B)
7.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10)
;
_shelx_res_checksum              53037
_shelx_fab_checksum              83291
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-08-24
_olex2_date_sample_submission    2016-08-19
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id 698o
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.135
_oxdiff_exptl_absorpt_empirical_full_min 0.910