Metal‒Organic Framework Supported Single Site Chromium(III) Catalyst for Ethylene Oligomerization at Low Pressure and Temperature
Goetjen, Timothy A.; Zhang, Xuan; Liu, Jian; Hupp, Joseph T.; Farha, Omar K.; ACS Sustainable Chemistry & Engineering 7 (2019) 2553–; doi:10.1021/acssuschemeng.8b05524

data_4515220
_publ_section_title
;
 Metal--Organic Framework Supported Single Site Chromium(III) Catalyst for
 Ethylene Oligomerization at Low Pressure and Temperature
;
_journal_issue                   2
_journal_name_full               'ACS Sustainable Chemistry &amp; Engineering'
_journal_page_first              2553
_journal_paper_doi               10.1021/acssuschemeng.8b05524
_journal_volume                  7
_journal_year                    2019
_chemical_formula_moiety         '0.08(C257.49 H120 Cl3 Cr3 O96 Zr18)'
_chemical_formula_sum            'C21.46 H10 Cl0.25 Cr0.25 O8 Zr1.5'
_chemical_formula_weight         554.48
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-10-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   39.100(2)
_cell_length_b                   39.100(2)
_cell_length_c                   16.7147(9)
_cell_measurement_reflns_used    6876
_cell_measurement_temperature    210
_cell_measurement_theta_max      61.801
_cell_measurement_theta_min      2.259
_cell_volume                     22130(2)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2017)'
_computing_data_collection       'APEX2 V2017.3 (Bruker, 2017)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      210.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.2081
_diffrn_reflns_av_unetI/netI     0.0681
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            88732
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        60.917
_diffrn_reflns_theta_max         60.917
_diffrn_reflns_theta_min         1.304
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    2.261
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.5553
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    0.499
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             3276
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.066
_exptl_crystal_size_min          0.063
_refine_diff_density_max         1.481
_refine_diff_density_min         -2.130
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.401
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         6316
_refine_ls_number_restraints     106
_refine_ls_restrained_S_all      1.434
_refine_ls_R_factor_all          0.1642
_refine_ls_R_factor_gt           0.1403
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3816
_refine_ls_wR_factor_ref         0.4006
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4217
_reflns_number_total             6316
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sc8b05524_si_002.cif
_cod_data_source_block           cr_sim_nu_1000_0m
_cod_original_cell_volume        22131(3)
_cod_original_formula_sum        'C21.46 H10 Cl0.25 Cr0.25 O8 Zr1.50'
_cod_database_code               4515220
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.871
_shelx_estimated_absorpt_t_min   0.686
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C10_$1-C10_$3
 1.4 with sigma of 0.02
 C11_$1-C11
 1.5 with sigma of 0.02
 Cr1-O1_$4
 2.158 with sigma of 0.02
 C9_$2-C9_$1
 2.48 with sigma of 0.02
3. Restrained planarity
 C12_$1, C8_$2, C9_$2, C10_$2, C10, C9, C8, C12, C8_$3, C9_$3, C10_$3, C10_$1,
 C8_$1, C9_$1
 with sigma of 0.1
 C12_$1, C8_$1, C9_$1, C10_$1, C10_$3, C9_$3, C8_$3, C12, C8, C9, C11, C10,
 C10_$2, C9_$2, C11_$1, C8_$2
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C11) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C5) \\sim Ueq,
Uanis(C4) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C7) \\sim
Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(Cl1A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C1) = Uanis(C2)
Uanis(C2) = Uanis(C7) = Uanis(C6) = Uanis(C5) = Uanis(C4) = Uanis(C3)
Uanis(C8) = Uanis(C12) = Uanis(C9) = Uanis(C11) = Uanis(C10)
5. Others
 Fixed Sof: H10(0.5) Cr1(0.125) Cl1A(0.125)
6.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C10(H10), C3(H3), C4(H4), C6(H6), C7(H7)
6.b Fitted hexagon refined as free rotating group:
 C3(C4,C5,C6,C7,C2)
;
_shelx_res_checksum              66919
_shelx_hkl_checksum              61752
_shelx_fab_checksum              42456
_olex2_submission_special_instructions 'No special instructions were received'