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_4003603
_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         'C90 H72 O20 Zr6, 2(C3 H7 N O), 2(Cl)'
_chemical_formula_sum            'C96 H86 Cl2 N2 O22 Zr6'
_chemical_formula_weight         2237.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 94.9340(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6473(3)
_cell_length_b                   19.6770(5)
_cell_length_c                   48.7602(12)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      46.20
_cell_measurement_theta_min      2.89
_cell_volume                     10177.7(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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0789
_diffrn_reflns_av_unetI/netI     0.0646
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            44594
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        46.355
_diffrn_reflns_theta_max         46.355
_diffrn_reflns_theta_min         1.819
_exptl_absorpt_coefficient_mu    5.895
_exptl_absorpt_correction_T_max  0.7491
_exptl_absorpt_correction_T_min  0.4848
_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            yellow
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_description       rod
_exptl_crystal_F_000             4504
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.178
_exptl_crystal_size_min          0.089
_refine_diff_density_max         1.103
_refine_diff_density_min         -1.081
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1017
_refine_ls_number_reflns         8671
_refine_ls_number_restraints     2550
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.1419
_refine_ls_R_factor_gt           0.1204
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+523.2305P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2506
_refine_ls_wR_factor_ref         0.2615
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6873
_reflns_number_total             8671
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm0c01965_si_011.cif
_cod_data_source_block           eric303_sq
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4003603
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.280
_shelx_estimated_absorpt_t_max   0.622
_shelx_res_checksum              11176
_shelx_hkl_checksum              79465
_shelx_fab_checksum              68078