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_7701970
_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 Cu10 F6 N48 Si'
_chemical_formula_sum            'C88 H96 Cu10 F6 N48 Si'
_chemical_formula_weight         2603.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc20nccf
_audit_creation_date             2019-10-06
_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                 111.0710(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.2435(2)
_cell_length_b                   26.0724(2)
_cell_length_c                   26.5968(2)
_cell_measurement_reflns_used    24067
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.6880
_cell_measurement_theta_min      3.6360
_cell_volume                     14393.2(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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.971
_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     42.00  85.00   0.50    5.00    --    0.00  38.00 120.00   86
  2  \w     34.00  71.00   0.50    5.00    --    0.00  19.00-120.00   74
  3  \w    -17.00  26.00   0.50    5.00    --    0.00  19.00-120.00   86
  4  \w     -5.00  29.00   0.50    5.00    --    0.00  38.00 120.00   68
  5  \w     88.00 116.00   0.50   40.00    --   89.30 -77.00  90.00   56
  6  \w      2.00  28.00   0.50   40.00    --   89.30 -61.00 120.00   52
  7  \w      0.00  37.00   0.50   40.00    --   89.30 -82.00  60.00   74
  8  \w      0.00  96.00   0.50   40.00    --   89.30 -30.00 120.00  192
  9  \w     70.00 110.00   0.50   40.00    --   89.30 -61.00 120.00   80
 10  \w     46.00 110.00   0.50   40.00    --   89.30 -82.00  60.00  128
 11  \w    114.00 175.00   0.50   40.00    --   89.30  61.00-120.00  122
 12  \w      1.00  40.00   0.50   40.00    --   89.30 -77.00  90.00   78
 13  \w     15.00  41.00   0.50   40.00    --   89.30 -61.00  60.00   52
 14  \w     61.00 107.00   0.50   40.00    --   89.30 -61.00  60.00   92
 15  \w      5.00 102.00   0.50   40.00    --   89.30 -30.00-150.00  194
;
_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      -0.0361456000
_diffrn_orient_matrix_UB_12      0.0427560000
_diffrn_orient_matrix_UB_13      0.0174427000
_diffrn_orient_matrix_UB_21      -0.0204186000
_diffrn_orient_matrix_UB_22      -0.0389031000
_diffrn_orient_matrix_UB_23      0.0344502000
_diffrn_orient_matrix_UB_31      0.0615322000
_diffrn_orient_matrix_UB_32      0.0122134000
_diffrn_orient_matrix_UB_33      0.0486044000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            39436
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.001
_diffrn_reflns_theta_min         3.562
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.138
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57393
_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    1.202
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             5272
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     710
_refine_ls_number_reflns         13495
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0348
_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^)+(0.0528P)^2^+17.9160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.0986
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12106
_reflns_number_total             13495
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04368c2.cif
_cod_data_source_block           cage2
_cod_database_code               7701970
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CNHCuSiFO
_reflns_odcompleteness_completeness 99.44
_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. Others
 Fixed Sof: F01N(0.5) F01T(0.5) F01Y(0.5) F022(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C01B(H01B,H01C), C01H(H01D,H01F), C01O(H01H,H01L), C023(H02A,H02B), C025(H02C,
 H02D), C026(H02E,H02F), C027(H02G,H02H), C029(H02I,H02J), C02B(H02K,H02L),
 C02E(H02N,H02O), C02G(H02P,H02Q), C02I(H02R,H02S)
3.b Aromatic/amide H refined with riding coordinates:
 C00U(H00U), C00Z(H00Z), C011(H011), C012(H012), C015(H015), C016(H016),
 C017(H017), C018(H018), C019(H019), C01A(H01A), C01E(H01E), C01G(H01G),
 C01I(H01I), C01J(H01J), C01K(H01K), C01P(H01P), C01Q(H01Q), C01R(H01R),
 C01U(H01U), C01W(H01W), C01X(H01X), C020(H020), C021(H021), C02C(H02M)
;
_shelx_res_checksum              76822
_shelx_fab_checksum              27033
_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 2.701
_oxdiff_exptl_absorpt_empirical_full_min 0.705