Coordination-Driven Self-Assembly of M10L8 Metal-Organic Bi-capped Square Antiprisms with Adaptable Cavity
Wang, Xue-Zhi; Sun, Meng-Ying; Zheng, Ji; Luo, Dong; Li, Qi; Zhou, Xiao-Ping; Li, Dan; Dalton Transactions  (2019) –; doi:10.1039/C9DT04368C

data_7701974
_publ_section_title
;
 Coordination-Driven Self-Assembly of M10L8 Metal-Organic Bi-capped Square
 Antiprisms with Adaptable Cavity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT04368C
_journal_year                    2019
_chemical_formula_moiety         'C88 H96 Br Cu10 N48'
_chemical_formula_sum            'C88 H96 Br Cu10 N48'
_chemical_formula_weight         2541.43
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc20ncdg
_audit_creation_date             2018-12-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-06 deposited with the CCDC.	2019-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.2461(2)
_cell_length_b                   19.2461(2)
_cell_length_c                   14.4823(3)
_cell_measurement_reflns_used    4065
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      71.8890
_cell_measurement_theta_min      3.2170
_cell_volume                     5364.42(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_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      100.00(11)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.968
_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    -56.00 -26.00   0.50    7.00    --    0.00 -57.00   1.00   60
  2  \w    103.00 128.00   0.50   13.00    --   96.10  64.00 -24.00   50
  3  \w    112.00 153.00   0.50   13.00    --   96.10  57.00 142.00   82
  4  \w    -32.00  36.00   0.50    7.00    --    0.00  82.00   0.00  136
  5  \w    112.00 172.00   0.50   13.00    --   96.10  77.00  90.00  120
  6  \w     82.00 115.00   0.50   13.00    --   96.10  38.00 120.00   66
  7  \w    133.00 180.00   0.50   13.00    --   96.10  38.00 120.00   94
  8  \w     97.00 182.00   0.50   13.00    --   96.10  82.00-180.00  170
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0782322000
_diffrn_orient_matrix_UB_12      -0.0167581000
_diffrn_orient_matrix_UB_13      0.0043531000
_diffrn_orient_matrix_UB_21      0.0135629000
_diffrn_orient_matrix_UB_22      -0.0517971000
_diffrn_orient_matrix_UB_23      0.0790943000
_diffrn_orient_matrix_UB_31      -0.0103632000
_diffrn_orient_matrix_UB_32      0.0586687000
_diffrn_orient_matrix_UB_33      0.0709634000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0594
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15561
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.346
_diffrn_reflns_theta_min         3.051
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    3.086
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       plate
_exptl_crystal_F_000             2570
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.787
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5222
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0491
_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^)+(0.0628P)^2^+5.6974P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1195
_refine_ls_wR_factor_ref         0.1310
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3731
_reflns_number_total             5222
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04368c2.cif
_cod_data_source_block           cage3
_cod_original_cell_volume        5364.42(16)
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               7701974
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         CNHOBrCu
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.970
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7a,H7b), C6(H6a,H6b), C5(H5a,H5b), C16(H16a,H16b), C18(H18a,H18b),
 C17(H17a,H17b)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C22(H22), C12(H12), C4(H4), C13(H13), C10(H10), C2(H2), C21(H21),
 C1(H1), C8(H8), C19(H19), C15(H15)
;
_shelx_res_checksum              52102
_shelx_fab_checksum              8770
_platon_squeeze_void_probe_radius 1.20
_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 1.081
_oxdiff_exptl_absorpt_empirical_full_min 0.915