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_4518616
_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 H61 N2 Ni O, C32 H12 B F24'
_chemical_formula_sum            'C91 H72 B F24 N2 Ni O'
_chemical_formula_weight         1735.02
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-02-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_cell_angle_alpha                109.732(2)
_cell_angle_beta                 101.015(2)
_cell_angle_gamma                110.139(2)
_cell_formula_units_Z            2
_cell_length_a                   16.7822(5)
_cell_length_b                   18.2187(6)
_cell_length_c                   18.2294(5)
_cell_measurement_reflns_used    62281
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.75
_cell_measurement_theta_min      1.84
_cell_volume                     4618.2(3)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.990
_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  0.0610
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            51495
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.324
_diffrn_reflns_theta_min         1.840
_exptl_absorpt_coefficient_mu    0.302
_exptl_absorpt_correction_T_max  0.9106
_exptl_absorpt_correction_T_min  0.6098
_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    1.248
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisma
_exptl_crystal_F_000             1778
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.367
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.649
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.0060(6)
_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   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1306
_refine_ls_number_reflns         16692
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0597
_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^)+(0.0828P)^2^+3.3555P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1528
_refine_ls_wR_factor_ref         0.1607
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13959
_reflns_number_total             16692
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c00778_si_005.cif
_cod_data_source_block           es473
_cod_database_code               4518616
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.915
_shelx_estimated_absorpt_t_min   0.864
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H15C)=Sof(H15D)=Sof(H13C)=Sof(H13D)=Sof(C14B)=Sof(H14B)=1-FVAR(1)
 Sof(H15A)=Sof(H15B)=Sof(H13A)=Sof(H13B)=Sof(C14A)=Sof(H14A)=FVAR(1)
 Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=
 Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=1-FVAR(2)
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C8)=
 Sof(H8A)=Sof(H8B)=Sof(H8C)=FVAR(2)
 Sof(F16A)=Sof(F17A)=Sof(F18A)=1-FVAR(3)
 Sof(F18)=Sof(F16)=Sof(F17)=FVAR(3)
 Sof(F14A)=Sof(F15A)=Sof(F13A)=1-FVAR(4)
 Sof(F15)=Sof(F13)=Sof(F14)=FVAR(4)
 Sof(F24A)=Sof(F23A)=Sof(F22A)=1-FVAR(5)
 Sof(F22)=Sof(F23)=Sof(F24)=FVAR(5)
 Sof(F5A)=Sof(F6A)=Sof(F4A)=1-FVAR(6)
 Sof(F6)=Sof(F5)=Sof(F4)=FVAR(6)
 Sof(F7A)=Sof(F9A)=Sof(F8A)=1-FVAR(7)
 Sof(F9)=Sof(F7)=Sof(F8)=FVAR(7)
 Sof(F1A)=Sof(F3A)=Sof(F2A)=1-FVAR(8)
 Sof(F3)=Sof(F2)=Sof(F1)=FVAR(8)
3.a Ternary CH refined with riding coordinates:
 C14A(H14A), C14B(H14B)
3.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C50(H50), C42(H42), C3(H3), C61(H61), C31(H31), C10(H10), C40(H40),
 C45(H45), C59(H59), C86(H86), C37(H37), C66(H66), C91(H91), C41(H41), C53(H53),
  C89(H89), C64(H64), C18(H18), C4(H4), C56(H56), C72(H72), C20(H20), C78(H78),
 C19(H19), C75(H75), C34(H34), C69(H69), C84(H84), C48(H48), C28(H28), C81(H81),
  C23(H23), C25(H25)
3.c X=CH2 refined with riding coordinates:
 C15(H15A,H15B), C15(H15C,H15D), C13(H13A,H13B), C13(H13C,H13D)
3.d Idealised Me refined as rotating group:
 C51(H51A,H51B,H51C), C33(H33A,H33B,H33C), C58(H58A,H58B,H58C), C47(H47A,H47B,
 H47C), C36(H36A,H36B,H36C), C55(H55A,H55B,H55C), C27(H27A,H27B,H27C), C7(H7A,
 H7B,H7C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C29(H29A,H29B,H29C), C7A(H7AA,H7AB,
 H7AC), C9A(H9AA,H9AB,H9AC), C8A(H8AA,H8AB,H8AC)
;
_olex2_submission_special_instructions 'No special instructions were received'