Ethylene Oligomerization in Metal‒Organic Frameworks Bearing Nickel(II) 2,2′-Bipyridine Complexes
Gonzalez, Miguel; Oktawiec, Julia; Long, Jeffrey R.; Faraday Discuss.  (2017) –; doi:10.1039/C7FD00061H

data_1545312
_publ_section_title
;
 Ethylene Oligomerization in Metal--Organic Frameworks Bearing Nickel(II)
 2,2&#x2032;-Bipyridine Complexes
;
_journal_name_full               'Faraday Discuss.'
_journal_paper_doi               10.1039/C7FD00061H
_journal_year                    2017
_chemical_formula_moiety
'C67.68 H33.84 Br11.28 N11.28 Ni5.64 O30.56 Zr6'
_chemical_formula_sum
'C67.68 H33.84 Br11.28 N11.28 Ni5.64 O30.56 Zr6'
_chemical_formula_weight         3277.67
_chemical_name_common            Zr6O4(OH)4(bpydc)5.64(NiBr2)5.64
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_Hall           '-P 2ac 2ab 3'
_space_group_name_H-M_alt        'P a -3'
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P a -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-01-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-02-03 deposited with the CCDC.
2017-02-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.2758(8)
_cell_length_b                   26.2758(8)
_cell_length_c                   26.2758(8)
_cell_measurement_reflns_used    9070
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.806
_cell_measurement_theta_min      2.366
_cell_volume                     18141.3(10)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 with PHOTON100 CMOS detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.8856
_diffrn_reflns_av_R_equivalents  0.0950
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            178387
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        29.806
_diffrn_reflns_theta_max         29.806
_diffrn_reflns_theta_min         2.160
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.130
_exptl_absorpt_correction_T_max  0.735
_exptl_absorpt_correction_T_min  0.606
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0923 before and 0.0708 after correction.
The Ratio of minimum to maximum transmission is 0.8244.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'yellow green'
_exptl_crystal_colour_primary    'yellow green'
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             6224
_exptl_crystal_size_max          0.0536
_exptl_crystal_size_mid          0.0536
_exptl_crystal_size_min          0.0536
_refine_diff_density_max         1.044
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         4662
_refine_ls_number_restraints     705
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0651
_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^)+(0.1011P)^2^+163.0712P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2002
_refine_ls_wR_factor_ref         0.2046
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4250
_reflns_number_total             4662
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7fd00061h2.cif
_cod_data_source_block           mig211s_sq
_cod_original_cell_volume        18141.3(17)
_cod_database_code               1545312
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.735
_shelx_estimated_absorpt_t_min   0.735
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.500(2) 0.500(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 C5-C4 \\sim C11-C10
 with sigma of 0.02
 C12-C11 \\sim C5-C6
 with sigma of 0.02
 N2-C12 \\sim N1-C6
 with sigma of 0.02
 N1-C2 \\sim N2-C8
 with sigma of 0.02
 C2-C3 \\sim C9-C8
 with sigma of 0.02
 C10-C12 \\sim C6-C4
 with sigma of 0.02
 C10-C8 \\sim C4-C2
 with sigma of 0.02
 C6-C4 \\sim C12-C10
 with sigma of 0.02
 C12-C8 \\sim C6-C2
 with sigma of 0.02
 C4-C2 \\sim C10-C8
 with sigma of 0.02
 C5-N1 \\sim N2-C11
 with sigma of 0.02
 N1-C3 \\sim N2-C9
 with sigma of 0.02
 C5-C3 \\sim C11-C9
 with sigma of 0.02
4. Restrained planarity
 N1, C1, C2, C3, C4, C5, C6, C12
 with sigma of 0.1
 N2, C6, C7, C8, C9, C10, C11, C12
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
O3 \\sim O4 \\sim O5 \\sim O6 \\sim N1 \\sim N2 \\sim C1 \\sim C2 \\sim C3
\\sim C4 \\sim H4 \\sim C5 \\sim H5 \\sim C6 \\sim C7 \\sim C8 \\sim H8 \\sim
C9 \\sim C10 \\sim H10 \\sim C11 \\sim H11 \\sim C12: within 2.6A with sigma of
0.04 and sigma for terminal atoms of 0.08
Ni1A \\sim Br1B \\sim Br2B \\sim Ni1B \\sim Br5A \\sim Br4A \\sim Br1A \\sim
Br2A \\sim Br3A: within 2.6A with sigma of 0.04 and sigma for terminal atoms of
0.08
O1A \\sim O2A \\sim O1B \\sim O2B: within 2.5A with sigma of 0.01 and sigma for
terminal atoms of 0.02
6. Rigid body (RIGU) restrains
 O3, O4, O5, N1, N2, C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3, O4, O5, O6, N1, N2, C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Ni1A, Br1B, Br2B, Ni1B, Br1A, Br2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Ni1A, Br1B, Br2B, Ni1B, Br4A, Br1A, Br2A, Br3A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Ni1A, Br1B, Br2B, Ni1B, Br5A, Br4A, Br1A, Br2A, Br3A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1A, O2A, O1B, O2B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Fixed Sof: O3(0.94) O4(0.94) O5(0.94) O6(0.94) N1(0.94) N2(0.94) C1(0.94)
 C2(0.94) H2(0.94) C3(0.94) C4(0.94) H4(0.94) C5(0.94) H5(0.94) C6(0.94)
 C7(0.94) C8(0.94) H8(0.94) C9(0.94) C10(0.94) H10(0.94) C11(0.94) H11(0.94)
 C12(0.94) Ni1A(0.64) O1A(0.5) O2A(0.16667) Br1B(0.3) Br2B(0.3) Ni1B(0.3)
 O1B(0.5) O2B(0.16667) Br4A(0.12) Br5A(0.12) Br1A(0.52) Br2A(0.4) Br3A(0.12)
8.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C8(H8), C10(H10), C11(H11)
;
_shelx_res_checksum              49110
_shelx_hkl_checksum              628
_shelx_fab_checksum              19086
_olex2_submission_special_instructions 'No special instructions were received'