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_7702238
_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
'1(C72 H84 Al6 Cu7 N12 O24), 6(Cl O4), 3(N0.67 O2), 21 (C H4 O)'
_chemical_formula_sum            'C93 H168 Al6 Cl6 Cu7 N14 O75'
_chemical_formula_weight         3501.76
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-11-07
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_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                   27.8468(6)
_cell_length_b                   27.8468(6)
_cell_length_c                   17.6945(7)
_cell_measurement_reflns_used    16493
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      27.1140
_cell_measurement_theta_min      3.7210
_cell_volume                     11882.8(6)
_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      120.01(10)
_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 0.998
_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    -20.00  33.00   1.00   20.00    --   -7.39 -99.00-180.00   53
  2  \w    -45.00   3.00   1.00   20.00    --   -7.39  95.00 -16.00   48
  3  \w    -20.00  49.00   1.00   20.00    --    8.80 -99.00   0.00   69
  4  \w    -65.00  40.00   1.00   20.00    --    8.80 -77.00 120.00  105
  5  \w     -5.00  77.00   1.00   20.00    --    8.80  38.00 -30.00   82
  6  \w      2.00  32.00   1.00   20.00    --    8.80 -57.00   0.00   30
  7  \w    -59.00  39.00   1.00   20.00    --    8.80 -19.00 150.00   98
;
_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      0.0086807000
_diffrn_orient_matrix_UB_12      -0.0039297000
_diffrn_orient_matrix_UB_13      -0.0360400000
_diffrn_orient_matrix_UB_21      -0.0260452000
_diffrn_orient_matrix_UB_22      -0.0243869000
_diffrn_orient_matrix_UB_23      -0.0051867000
_diffrn_orient_matrix_UB_31      -0.0105685000
_diffrn_orient_matrix_UB_32      0.0159508000
_diffrn_orient_matrix_UB_33      -0.0167713000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            49850
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.345
_diffrn_reflns_theta_min         2.856
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.151
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8957
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0596 before and 0.0518 after correction.
The Ratio of minimum to maximum transmission is 0.8957.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_description       block
_exptl_crystal_F_000             5421
_exptl_crystal_recrystallization_method
'The material was recrystallised from methanol by slow evaporation'
_exptl_crystal_size_max          0.318
_exptl_crystal_size_mid          0.243
_exptl_crystal_size_min          0.165
_refine_diff_density_max         1.219
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         4843
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0561
_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^)+(0.0895P)^2^+80.5735P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1635
_refine_ls_wR_factor_ref         0.1697
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4209
_reflns_number_total             4843
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03793k2.cif
_cod_data_source_block           7
_cod_original_cell_volume        11882.8(7)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7702238
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C30 H30 N10 O10 Cu Al'
_chemical_oxdiff_usercomment     '@ 120 K 792o SE'
_shelx_estimated_absorpt_t_max   0.833
_shelx_estimated_absorpt_t_min   0.711
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
2. Restrained distances
 O4-H4 = O3-H3
 0.84 with sigma of 0.02
 O104-N101 = O103-N101
 1.25 with sigma of 0.02
 O6-O7 \\sim O6-O8 \\sim O8A-O6A \\sim O6A-O7A
 with sigma of 0.04
 Cl1-O5 \\sim Cl1-O6 \\sim Cl1-O7 \\sim Cl1-O8 \\sim Cl1-O8A \\sim Cl1-O6A
\\sim Cl1-O7A
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 Cl1, O5, O6, O6A, O7, O7A, O8, O8A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O103, O104, N101
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O6A)=Sof(O7A)=Sof(O8A)=1-FVAR(1)
 Sof(O6)=Sof(O7)=Sof(O8)=FVAR(1)
 Fixed Sof: O103(0.6666) O104(0.33333) N101(0.33333)
5.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3A), C4(H4A), C7(H7), C8(H8), C9(H9), C10(H10)
;
_shelx_res_checksum              10992
_shelx_fab_checksum              46864
_olex2_date_sample_data_collection 2017-01-11
_olex2_date_sample_submission    2017-01-11
_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 '792o SE'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.211
_oxdiff_exptl_absorpt_empirical_full_min 0.865