The Impact of Charge in a Ni(II) Polymerization Catalyst
Schiebel, Eva; Voccia, Maria; Falivene, Laura; Caporaso, Lucia; Mecking, Stefan; ACS Catalysis  (2021) 5358–5368; doi:10.1021/acscatal.1c00778

data_4518613
_publ_section_title
;
 The Impact of Charge in a Ni(II) Polymerization Catalyst
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              5358
_journal_page_last               5368
_journal_paper_doi               10.1021/acscatal.1c00778
_journal_year                    2021
_chemical_formula_moiety         'C59 H33 F24 N3 Ni O, C32 H12 B F24'
_chemical_formula_sum            'C91 H45 B F48 N3 Ni O'
_chemical_formula_weight         2177.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-09-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 107.621(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   44.1023(14)
_cell_length_b                   11.9357(4)
_cell_length_c                   37.7488(10)
_cell_measurement_reflns_used    45610
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.60
_cell_measurement_theta_min      1.77
_cell_volume                     18938.3(10)
_computing_cell_refinement       'X-Area Recipe 1.33.0.0 (STOE, 2015)'
_computing_data_collection       'X-Area WinXpose 2.0.22.0 (STOE, 2016)'
_computing_data_reduction
;
X-Area Integrate 1.74.2.0 (STOE, 2018)
X-Area LANA 1.75.3.0 (STOE, 2018)
;
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
 360 frames, detector distance = 110 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1151
_diffrn_reflns_av_unetI/netI     0.0655
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            99181
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.389
_diffrn_reflns_theta_min         1.698
_exptl_absorpt_coefficient_mu    0.347
_exptl_absorpt_correction_T_max  0.9611
_exptl_absorpt_correction_T_min  0.3536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             8680
_exptl_crystal_recrystallization_method 'Methylene chloride/pentane layered'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.328
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.00037(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1453
_refine_ls_number_reflns         17175
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1151
_refine_ls_R_factor_gt           0.0703
_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^)+(0.1040P)^2^+30.2771P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1823
_refine_ls_wR_factor_ref         0.2087
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10287
_reflns_number_total             17175
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c00778_si_002.cif
_cod_data_source_block           es484_2
_cod_database_code               4518613
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F12A-C59 \\sim F10B-C59
 with sigma of 0.02
 F10A-C59 \\sim F11B-C59
 with sigma of 0.02
 F11A-C59 \\sim F12B-C59
 with sigma of 0.02
 F49-C79 \\sim F36-C79
 with sigma of 0.02
 F10-C79 \\sim F35-C79
 with sigma of 0.02
 F11-C79 \\sim F34-C79
 with sigma of 0.02
 C25-F16 \\sim C25-F16A
 with sigma of 0.02
 C25-F18 \\sim C25-F18A
 with sigma of 0.02
 F17-C25 \\sim F12-C25
 with sigma of 0.02
 C66-F48 \\sim C66-F48A
 with sigma of 0.02
 C66-F47 \\sim C66-F47A
 with sigma of 0.02
 C66-F46 \\sim C66-F46A
 with sigma of 0.02
3. Others
 Sof(F39)=Sof(F37)=Sof(F38)=1-FVAR(1)
 Sof(F03S)=Sof(F03T)=Sof(F03X)=FVAR(1)
 Sof(F11B)=Sof(F10B)=Sof(F12B)=1-FVAR(2)
 Sof(F11A)=Sof(F12A)=Sof(F10A)=FVAR(2)
 Sof(F36)=Sof(F34)=Sof(F35)=1-FVAR(3)
 Sof(F49)=Sof(F11)=Sof(F10)=FVAR(3)
 Sof(F12)=Sof(F16A)=Sof(F18A)=1-FVAR(4)
 Sof(F17)=Sof(F16)=Sof(F18)=FVAR(4)
 Sof(F47A)=Sof(F48A)=Sof(F46A)=1-FVAR(5)
 Sof(F48)=Sof(F47)=Sof(F46)=FVAR(5)
4.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C91(H91), C85(H85), C6(H6), C3(H3), C51(H51), C20(H20), C31(H31),
 C75(H75), C37(H37), C18(H18), C69(H69), C19(H19), C67(H67), C72(H72), C83(H83),
  C77(H77), C8(H8), C15(H15), C61(H61), C40(H40), C29(H29), C42(H42), C11(H11),
 C58(H58), C34(H34), C53(H53), C80(H80), C88(H88), C56(H56), C45(H45), C41(H41),
  C26(H26), C23(H23), C13(H13), C48(H48), C12(H12), C64(H64)
4.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C10(H10A,H10B,H10C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              40974
_shelx_hkl_checksum              56454
_shelx_fab_checksum              87613
_olex2_submission_special_instructions 'No special instructions were received'