Ethylene polymerization with a crystallographically well-defined metal–organic framework supported catalyst
Goetjen, Timothy A.; Knapp, Julia G.; Syed, Zoha H.; Hackler, Ryan A.; Zhang, Xuan; Delferro, Massimiliano; Hupp, Joseph T.; Farha, Omar K.; Catalysis Science & Technology 12 (2022) 1619–1627; doi:10.1039/D1CY01990B

data_1566239
_publ_section_title
;
 Ethylene polymerization with a crystallographically well-defined
 metal--organic framework supported catalyst
;
_journal_issue                   5
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              1619
_journal_page_last               1627
_journal_paper_doi               10.1039/D1CY01990B
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C45.269 H22 Al Cl2 Cr0.184 O15.333 Zr3'
_chemical_formula_sum            'C45.27 H22 Al Cl2 Cr0.18 O15.33 Zr3'
_chemical_formula_weight         1192.25
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_audit_update_record
;
2021-10-11 deposited with the CCDC.	2021-12-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   39.433(3)
_cell_length_b                   39.433(3)
_cell_length_c                   16.2564(5)
_cell_measurement_reflns_used    8019
_cell_measurement_temperature    200.15
_cell_measurement_theta_max      49.55
_cell_measurement_theta_min      2.23
_cell_volume                     21891(2)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      200.15
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker SMART CCD 1K area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'f\ and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1309
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            29356
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        39.973
_diffrn_reflns_theta_max         39.973
_diffrn_reflns_theta_min         3.424
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    2.419
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.799
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'clear greenish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.543
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3526
_exptl_crystal_recrystallization_method 'Crystal is rod shaped.'
_exptl_crystal_size_max          0.101
_exptl_crystal_size_mid          0.039
_exptl_crystal_size_min          0.018
_refine_diff_density_max         0.551
_refine_diff_density_min         -1.220
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         2583
_refine_ls_number_restraints     246
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1033
_refine_ls_R_factor_gt           0.0859
_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^)+(0.1999P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2454
_refine_ls_wR_factor_ref         0.2678
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1768
_reflns_number_total             2583
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cy01990b2.cif
_cod_data_source_block           DEAC@Cr-SIM-NU-1000_audit_creation_date
_cod_depositor_comments          'Adding full bibliography for 1566239.cif.'
_cod_original_cell_volume        21891(3)
_cod_database_code               1566239
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.792
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C12-C12_$3
 1.4 with sigma of 0.02
 C12-C10_$2
 1.4 with sigma of 0.02
 O4-Al9
 1.918 with sigma of 0.02
 O4_$4-Al9
 1.918 with sigma of 0.02
 C8-C5 \\sim C8-C6
 with sigma of 0.02
 O7-C1 \\sim O5-C1
 with sigma of 0.02
3. Restrained planarity
 C8, C9, C10, C11, C12
 with sigma of 0.1
 C8_$1, C8_$3, C8_$2, C8, C9_$3, C9, C10_$2, C10, C10_$3, C10_$1, C11, C11_$3,
 C11_$1, C11_$2, C12_$3, C12
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: O4(0.33335)
7.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C4(H4), C3(H3), C5(H5), C9(H9), C11(H11)
7.b Fitted hexagon refined as free rotating group:
 C7(C6,C4,C2,C3,C5)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              99487
_shelx_fab_checksum              12853
_olex2_submission_special_instructions 'No special instructions were received'