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_4003609
_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         'C66 H57 F3 O20 Zr6, 2(Cl)'
_chemical_formula_sum            'C66 H57 Cl2 F3 O20 Zr6'
_chemical_formula_weight         1845.33
_space_group_crystal_system      hexagonal
_space_group_IT_number           190
_space_group_name_Hall           'P -6c -2c'
_space_group_name_H-M_alt        'P -6 2 c'
_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                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   16.4279(9)
_cell_length_b                   16.4279(9)
_cell_length_c                   21.9721(19)
_cell_measurement_reflns_used    2193
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      74.67
_cell_measurement_theta_min      3.70
_cell_volume                     5135.3(6)
_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      150(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0299
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            36400
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.794
_diffrn_reflns_theta_min         3.106
_exptl_absorpt_coefficient_mu    5.757
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.5044
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_description       block
_exptl_crystal_F_000             1828
_exptl_crystal_size_max          0.407
_exptl_crystal_size_mid          0.237
_exptl_crystal_size_min          0.226
_refine_diff_density_max         3.762
_refine_diff_density_min         -1.147
_refine_diff_density_rms         0.231
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.34(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.277
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         3616
_refine_ls_number_restraints     289
_refine_ls_restrained_S_all      1.256
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0885
_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^)+(0.1669P)^2^+7.5273P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2477
_refine_ls_wR_factor_ref         0.2514
_reflns_Friedel_coverage         0.800
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                3523
_reflns_number_total             3616
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm0c01965_si_010.cif
_cod_data_source_block           eric316a_sq
_cod_original_cell_volume        5135.3(7)
_cod_database_code               4003609
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.203
_shelx_estimated_absorpt_t_max   0.356
_shelx_res_checksum              58403
_shelx_hkl_checksum              73743
_shelx_fab_checksum              20529