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_7701975
_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         'C22 H26 Cu2 N12, F6 Si'
_chemical_formula_sum            'C22 H26 Cu2 F6 N12 Si'
_chemical_formula_weight         727.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc20nchk
_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                 93.0570(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.61500(10)
_cell_length_b                   14.2500(2)
_cell_length_c                   10.57550(10)
_cell_measurement_reflns_used    5191
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.9220
_cell_measurement_theta_min      4.1770
_cell_volume                     1296.44(3)
_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 0.969
_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  43.00   0.50    0.50    --    0.00  38.00 120.00  118
  2  \w     50.00  89.00   0.50    0.50    --    0.00  38.00 120.00   78
  3  \w    -87.00 -49.00   0.50    0.50    --    0.00 -19.00-150.00   76
  4  \w      8.00  40.00   0.50    0.50    --   95.80 -15.00 150.00   64
  5  \w     22.00 107.00   0.50    0.50    --   95.80 -45.00  60.00  170
  6  \w     23.00 104.00   0.50    0.50    --   95.80 -30.00-120.00  162
  7  \w     28.00  87.00   0.50    0.50    --   95.80 -30.00  90.00  118
  8  \w     47.00 117.00   0.50    0.50    --   95.80 -15.00 150.00  140
  9  \w      7.00  73.00   0.50    0.50    --   95.80 -15.00  30.00  132
 10  \w      6.00 118.00   0.50    0.50    --   95.80 -15.00 -90.00  224
;
_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      0.0677781000
_diffrn_orient_matrix_UB_12      -0.0463051000
_diffrn_orient_matrix_UB_13      -0.1165564000
_diffrn_orient_matrix_UB_21      0.1414184000
_diffrn_orient_matrix_UB_22      0.0661628000
_diffrn_orient_matrix_UB_23      0.0126490000
_diffrn_orient_matrix_UB_31      0.0864495000
_diffrn_orient_matrix_UB_32      -0.0718801000
_diffrn_orient_matrix_UB_33      0.0868102000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0124
_diffrn_reflns_av_unetI/netI     0.0130
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6081
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.256
_diffrn_reflns_theta_min         5.141
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.235
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83229
_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    1.864
_exptl_crystal_description       needle
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2563
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0283
_refine_ls_R_factor_gt           0.0280
_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^)+(0.0410P)^2^+1.4896P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0745
_refine_ls_wR_factor_ref         0.0748
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2532
_reflns_number_total             2563
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04368c2.cif
_cod_data_source_block           CP6
_cod_database_code               7701975
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CNHCuF
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.938
_reflns_odcompleteness_completeness 99.84
_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, All N(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7a,H7b), C6(H6a,H6b), C5(H5a,H5b)
2.b Aromatic/amide H refined with riding coordinates:
 N5(H5), C4(H4), C1(H1), C8(H8), C2(H2), C11(H11), C10(H10)
;
_shelx_res_checksum              63192
_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 1.285
_oxdiff_exptl_absorpt_empirical_full_min 0.748