Ligand-Based Phase Control in Porous Zirconium Coordination Cages
Gosselin, Eric J.; Decker, Gerald E.; McNichols, Brett W.; Baumann, James E.; Yap, Glenn P. A.; Sellinger, Alan; Bloch, Eric D.; Chemistry of Materials  (2020) –; doi:10.1021/acs.chemmater.0c01965

data_4003602
_publ_section_title
;
 Ligand-Based Phase Control in Porous Zirconium Coordination Cages
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.0c01965
_journal_year                    2020
_chemical_formula_moiety         'C96 H84 O20 Zr6, 4(C3 H7 N O), 2(Cl)'
_chemical_formula_sum            'C108 H112 Cl2 N4 O24 Zr6'
_chemical_formula_weight         2468.23
_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
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 102.424(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.921(3)
_cell_length_b                   16.858(2)
_cell_length_c                   31.905(4)
_cell_measurement_reflns_used    2708
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      39.63
_cell_measurement_theta_min      2.84
_cell_volume                     12039(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker AXS APEX diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1145
_diffrn_reflns_av_unetI/netI     0.0779
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            21135
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        40.047
_diffrn_reflns_theta_max         40.047
_diffrn_reflns_theta_min         2.836
_exptl_absorpt_coefficient_mu    5.052
_exptl_absorpt_correction_T_max  0.7479
_exptl_absorpt_correction_T_min  0.5862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_description       block
_exptl_crystal_F_000             5016
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.074
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     648
_refine_ls_number_reflns         3649
_refine_ls_number_restraints     1552
_refine_ls_restrained_S_all      0.887
_refine_ls_R_factor_all          0.0995
_refine_ls_R_factor_gt           0.0532
_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^)+(0.0792P)^2^+63.3583P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1481
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2340
_reflns_number_total             3649
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm0c01965_si_013.cif
_cod_data_source_block           eric338_sq
_cod_original_cell_volume        12040(2)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4003602
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.560
_shelx_estimated_absorpt_t_max   0.706
_shelx_res_checksum              12588
_shelx_hkl_checksum              69936
_shelx_fab_checksum              49166