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_4003604
_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         'C60 H54 O20 S3 Zr6, 2(C3 H7 N O), 2(Cl)'
_chemical_formula_sum            'C66 H68 Cl2 N2 O22 S3 Zr6'
_chemical_formula_weight         1955.62
_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                 90.483(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   39.7702(12)
_cell_length_b                   22.4499(7)
_cell_length_c                   10.8784(3)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      59.06
_cell_measurement_theta_min      3.87
_cell_volume                     9712.3(5)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0399
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            37630
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        59.044
_diffrn_reflns_theta_max         59.044
_diffrn_reflns_theta_min         2.222
_exptl_absorpt_coefficient_mu    6.680
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.5464
_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_colour            colourless
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       plate
_exptl_crystal_F_000             3904
_exptl_crystal_size_max          0.154
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.085
_refine_diff_density_max         1.905
_refine_diff_density_min         -1.419
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         6962
_refine_ls_number_restraints     522
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0545
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0818P)^2^+111.3408P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1418
_refine_ls_wR_factor_ref         0.1507
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5932
_reflns_number_total             6962
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm0c01965_si_009.cif
_cod_data_source_block           eric312_sq
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4003604
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.426
_shelx_estimated_absorpt_t_max   0.601
_shelx_res_checksum              63260
_shelx_hkl_checksum              17219
_shelx_fab_checksum              40766