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_7702239
_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 Cr2 Fe5 N12 O12, 4(Cl1 O4), 9 C H4 O'
_chemical_formula_sum            'C81 H108 Cl4 Cr2 Fe5 N12 O37'
_chemical_formula_weight         2366.84
_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             2016-12-06
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_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                   14.6087(3)
_cell_length_b                   14.6087(3)
_cell_length_c                   37.9381(19)
_cell_measurement_reflns_used    7747
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      73.0590
_cell_measurement_theta_min      4.1670
_cell_volume                     7011.8(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43h (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43h (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43h (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 1.0000
_diffrn_measured_fraction_theta_max 0.9900
_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    -96.00  -2.00   1.00   15.00    --  -43.17 125.00  30.00   94
  2  \w    -96.00  -2.00   1.00   15.00    --  -43.17 125.00 120.00   94
  3  \w   -116.00 -21.00   1.00   15.00    --  -43.17 -38.00  30.00   95
  4  \w   -116.00 -21.00   1.00   15.00    --  -43.17 -38.00 -60.00   95
  5  \w      1.00  83.00   1.00   15.00    --   43.17 -99.00 -90.00   82
  6  \w     30.00 109.00   1.00   25.00    --  111.00 -94.00-120.00   79
  7  \w     87.00 178.00   1.00   25.00    --  111.00  45.00 -60.00   91
  8  \w     41.00 139.00   1.00   25.00    --  111.00 -61.00   0.00   98
  9  \w     38.00 118.00   1.00   25.00    --  111.00-118.00 141.00   80
 10  \w     37.00 142.00   1.00   25.00    --  111.00 -77.00-120.00  105
 11  \w     36.00 135.00   1.00   25.00    --  111.00 -30.00 -30.00   99
 12  \w     39.00 121.00   1.00   25.00    --  111.00-125.00  30.00   82
 13  \w     87.00 178.00   1.00   25.00    --  111.00  45.00 -30.00   91
 14  \w     40.00 135.00   1.00   25.00    --  111.00 -45.00  90.00   95
 15  \w     41.00 139.00   1.00   25.00    --  111.00 -61.00-150.00   98
 16  \w     30.00 109.00   1.00   25.00    --  111.00 -94.00   0.00   79
 17  \w     87.00 178.00   1.00   25.00    --  111.00  30.00 -90.00   91
 18  \w     30.00 109.00   1.00   25.00    --  111.00 -94.00  30.00   79
 19  \w     39.00 121.00   1.00   25.00    --  111.00-125.00-150.00   82
 20  \w     87.00 178.00   1.00   25.00    --  111.00  45.00   0.00   91
 21  \w     39.00 121.00   1.00   25.00    --  111.00-125.00 120.00   82
 22  \w     84.00 116.00   1.00   25.00    --  111.00-125.00   0.00   32
 23  \w     45.00 120.00   1.00   25.00    --  111.00-125.00-180.00   75
 24  \w     47.00 121.00   1.00   25.00    --  111.00-125.00-120.00   74
 25  \w    108.00 171.00   1.00   25.00    --  111.00  15.00  60.00   63
;
_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      0.0052394000
_diffrn_orient_matrix_UB_12      0.0192787000
_diffrn_orient_matrix_UB_13      -0.0400609000
_diffrn_orient_matrix_UB_21      0.0822667000
_diffrn_orient_matrix_UB_22      -0.0360845000
_diffrn_orient_matrix_UB_23      -0.0035575000
_diffrn_orient_matrix_UB_31      -0.0896489000
_diffrn_orient_matrix_UB_32      -0.1146778000
_diffrn_orient_matrix_UB_33      -0.0055940000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0968
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            32839
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.728
_diffrn_reflns_theta_min         3.495
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    9.765
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.731
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43h (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale brown'
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_description       plate
_exptl_crystal_F_000             3660
_exptl_crystal_recrystallization_method
'The material was recrystallised from methanol by hydrothermal bomb'
_exptl_crystal_size_max          0.139
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.033
_platon_squeeze_details          '9 MeOH per wheel'
_refine_diff_density_max         1.455
_refine_diff_density_min         -1.027
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3272
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0712
_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^)+(0.1458P)^2^+13.1062P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2052
_refine_ls_wR_factor_ref         0.2197
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2673
_reflns_number_total             3272
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03793k2.cif
_cod_data_source_block           2
_cod_original_cell_volume        7011.8(5)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7702239
_chemical_oxdiff_formula         'C30 H30 N10 O10 Cr2 Fe5 Cl2'
_chemical_oxdiff_usercomment     '@ 120 K 788o '
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{Fe1, Cr1}
3. Restrained distances
 O4-O3 \\sim O5-O6
 with sigma of 0.02
 Cl1-O3 \\sim Cl1-O4 \\sim Cl1-O3A
 with sigma of 0.02
 Cl1-O3 \\sim Cl1-O4 \\sim Cl1-O3A \\sim Cl1-O4A
 with sigma of 0.02
 O4A-O3A \\sim O3-O4
 with sigma of 0.02
 Cl2-O5 \\sim Cl2-O6
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(Fe1) = Uanis(Cr1)
5. Rigid body (RIGU) restrains
 Cl2, O5, O6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1, O3A, O4, O3, O4A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O3A)=1-FVAR(1)
 Sof(O4A)=0.3333*(1-FVAR(2))
 Sof(O4)=0.33333*FVAR(2)
 Sof(O3)=FVAR(1)
 Fixed Sof: Fe1(0.66667) Cr1(0.3333)
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              54276
_shelx_fab_checksum              75641
_shelx_shelxl_version_number     2016/6
_olex2_date_sample_data_collection 2016-11-24
_olex2_date_sample_submission    2016-11-21
_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 788o
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.009
_oxdiff_exptl_absorpt_empirical_full_min 0.575
_platon_squeeze_void_probe_radius 1.20