Metalation Triggers Single Crystalline Order in a Porous Solid.
Hou, Yun-Long; Yee, Ka-Kit; Wong, Yan-Lung; Zha, Meiqin; He, Jun; Zeller, Matthias; Hunter, Allen D.; Yang, Kaiqi; Xu, Zhengtao; Journal of the American Chemical Society 138 (2016) 14852–14855; doi:10.1021/jacs.6b09763

data_4131135
_publ_section_title
;
 Metalation Triggers Single Crystalline Order in a Porous Solid.
;
_journal_issue                   45
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14852
_journal_page_last               14855
_journal_paper_doi               10.1021/jacs.6b09763
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety
'C202.54 H242.54 Cl15.22 Hg7.60 O44 S36 Zr6, 3.984(C2 H3 N), 3(O)'
_chemical_formula_sum
'C214.51 H260.49 Cl15.22 Hg7.61 N5.98 O47 S36 Zr6'
_chemical_formula_weight         7441.66
_space_group_crystal_system      cubic
_space_group_IT_number           201
_space_group_name_Hall           '-P 2ab 2bc 3'
_space_group_name_H-M_alt        'P n -3 :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.6473(15)
_cell_length_b                   33.6473(15)
_cell_length_c                   33.6473(15)
_cell_measurement_reflns_used    9654
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.9682
_cell_measurement_theta_min      2.4963
_cell_volume                     38093(3)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2014)'
_computing_data_collection       'Apex2 v2014.11 (Bruker, 2014)'
_computing_data_reduction        'SAINT V8.34A (Bruker, 2014)'
_computing_structure_refinement
;  
SHELXL-2014/7 (Sheldrick, 2014), 
SHELXLE Rev714 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker AXS D8 Quest CMOS diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'laterally graded multilayer (Goebel) mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1062
_diffrn_reflns_av_unetI/netI     0.0798
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            127861
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.323
_diffrn_reflns_theta_min         2.182
_diffrn_source                   'I-mu-S microsource X-ray tube'
_exptl_absorpt_coefficient_mu    3.561
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 v2014.11 (Bruker, 2014)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_description       prism
_exptl_crystal_F_000             14595
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.290
_refine_diff_density_max         4.502
_refine_diff_density_min         -1.881
_refine_diff_density_rms         0.255
_refine_ls_extinction_coef       0.00103(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         15812
_refine_ls_number_restraints     716
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.2185
_refine_ls_R_factor_gt           0.1280
_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^)+(0.1762P)^2^+706.7275P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3212
_refine_ls_wR_factor_ref         0.3957
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8522
_reflns_number_total             15812
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b09763_si_002.cif
_cod_data_source_block           Quest15mz306_0m
_cod_original_cell_volume        38093(5)
_cod_original_sg_symbol_H-M      'P n -3'
_cod_database_code               4131135
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.323
_shelx_estimated_absorpt_t_max   0.425
_shelx_res_checksum              17760
_shelx_hkl_checksum              56134