Control the Structure of Zr-Tetracarboxylate Frameworks through Steric Tuning.
Pang, Jiandong; Yuan, Shuai; Qin, Junsheng; Liu, Caiping; Lollar, Christina; Wu, Mingyan; Yuan, Daqiang; Zhou, Hong-Cai; Hong, Maochun; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b09973

data_4126731
_publ_section_title
;
 Control the Structure of Zr-Tetracarboxylate Frameworks through Steric
 Tuning.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b09973
_journal_year                    2017
_chemical_formula_sum            'C44.67 H44 O16.67 Zr3'
_chemical_formula_weight         1121.22
_space_group_crystal_system      hexagonal
_space_group_IT_number           191
_space_group_name_Hall           '-P 6 2'
_space_group_name_H-M_alt        'P 6/m m m'
_symmetry_space_group_name_Hall  '-P 6 2'
_symmetry_space_group_name_H-M   'P 6/m m m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   40.4113(11)
_cell_length_b                   40.4113(11)
_cell_length_c                   15.6898(6)
_cell_measurement_reflns_used    7751
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      48.8531
_cell_measurement_theta_min      2.8164
_cell_volume                     22189.8(12)
_computing_cell_refinement       'SAINT+ ver. (Bruker, 2001)'
_computing_data_collection       'APEX2  (Bruker, 2008)'
_computing_data_reduction        'SAINT+ ver. (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.2198
_diffrn_reflns_av_unetI/netI     0.1255
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       42
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_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5992
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        59.135
_diffrn_reflns_theta_max         59.135
_diffrn_reflns_theta_min         2.187
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.893
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.5117
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.503
_exptl_crystal_description       Block
_exptl_crystal_F_000             3392
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.782
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         5992
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.784
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0369P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0878
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2735
_reflns_number_total             5992
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b09973_si_002.cif
_cod_data_source_block           MLPCN-608-2
_cod_original_cell_volume        22189.8(15)
_cod_database_code               4126731
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              12358
_shelx_hkl_checksum              97018
_shelx_fab_checksum              82136