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_7701971
_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         '0.5(C44 H50 Cu4 N24), Cl O4'
_chemical_formula_sum            'C22 H25 Cl Cu2 N12 O4'
_chemical_formula_weight         684.07
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc20ncgj
_audit_creation_date             2019-08-21
_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            4
_cell_length_a                   9.4211(5)
_cell_length_b                   14.8334(5)
_cell_length_c                   21.6671(10)
_cell_measurement_reflns_used    4309
_cell_measurement_temperature    100
_cell_measurement_theta_max      70.4800
_cell_measurement_theta_min      5.5440
_cell_volume                     3027.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (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_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.981
_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    -16.00  32.00   0.50    1.50    --    0.00  38.00   0.00   96
  2  \w     54.00  89.00   0.50    1.50    --    0.00  38.00  90.00   70
  3  \w    -17.00  50.00   0.50    1.50    --    0.00  38.00  90.00  134
  4  \w     55.00  80.00   0.50    1.50    --    0.00  38.00   0.00   50
  5  \w     29.00 120.00   0.50    6.00    --   89.30 -82.00 -90.00  182
  6  \w     78.00 179.00   0.50    6.00    --   89.30  30.00 120.00  202
  7  \w    113.00 169.00   0.50    6.00    --   89.30  61.00  30.00  112
  8  \w     66.00 105.00   0.50    6.00    --   89.30  61.00  30.00   78
  9  \w     50.00 102.00   0.50    6.00    --   89.30 -82.00-150.00  104
 10  \w     66.00 143.00   0.50    6.00    --   89.30  61.00  60.00  154
 11  \w      5.00 113.00   0.50    6.00    --   89.30 -61.00 -90.00  216
;
_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      -0.1043711000
_diffrn_orient_matrix_UB_12      0.0413773000
_diffrn_orient_matrix_UB_13      0.0467894000
_diffrn_orient_matrix_UB_21      0.1225223000
_diffrn_orient_matrix_UB_22      0.0142426000
_diffrn_orient_matrix_UB_23      0.0460866000
_diffrn_orient_matrix_UB_31      0.0273893000
_diffrn_orient_matrix_UB_32      0.0942591000
_diffrn_orient_matrix_UB_33      -0.0274211000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0772
_diffrn_reflns_av_unetI/netI     0.0613
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            14261
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.109
_diffrn_reflns_theta_min         4.081
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.968
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49278
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_description       plank
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.675
_refine_diff_density_min         -0.970
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         2886
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0660
_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/[\s^2^(Fo^2^)+(0.0984P)^2^+4.8361P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1807
_refine_ls_wR_factor_ref         0.1918
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2302
_reflns_number_total             2886
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04368c2.cif
_cod_data_source_block           CP5
_cod_database_code               7701971
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C N O H Cu Cl'
_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.756
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Others
 Fixed Sof: H1(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C7(H7A,H7B), C6(H6A,H6B)
3.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C11(H11), C10(H10), C1(H1A), C4(H4), C8(H8), C2(H2)
;
_shelx_res_checksum              7579
_shelx_fab_checksum              31037
_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 1.850
_oxdiff_exptl_absorpt_empirical_full_min 0.342