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_4518615
_publ_section_title
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 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         'C56 H30.7 F24 N2 Ni O'
_chemical_formula_sum            'C56 H31 F24 N2 Ni O'
_chemical_formula_weight         1262.54
_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   geom
_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                88.69
_cell_angle_beta                 69.98
_cell_angle_gamma                65.61
_cell_formula_units_Z            2
_cell_length_a                   13.606
_cell_length_b                   13.645
_cell_length_c                   17.543
_cell_measurement_reflns_used    44114
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.63
_cell_measurement_theta_min      1.72
_cell_volume                     2760.166
_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      100.0
_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 0.976
_diffrn_measurement_details
;
 360 frames, detector distance = 100 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  0.0413
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            45030
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.393
_diffrn_reflns_theta_min         1.655
_exptl_absorpt_coefficient_mu    0.474
_exptl_absorpt_correction_T_max  0.9734
_exptl_absorpt_correction_T_min  0.5780
_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    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1266
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.027
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.883
_refine_diff_density_rms         0.122
_refine_ls_extinction_coef       0.0181(14)
_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   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     881
_refine_ls_number_reflns         14880
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0595
_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^)+(0.1106P)^2^+0.8529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1657
_refine_ls_wR_factor_ref         0.1818
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11152
_reflns_number_total             14880
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c00778_si_003.cif
_cod_data_source_block           esrs08
_cod_original_cell_volume        2760.0
_cod_database_code               4518615
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C10, C10A}
{C12, C12A}
3. Restrained distances
 C30-F9 \\sim C30-F8A
 with sigma of 0.02
 C30-F8 \\sim C30-F7A
 with sigma of 0.02
 C44-F13A \\sim C44-F14
 with sigma of 0.02
 C30-F7 \\sim C30-F9A
 with sigma of 0.02
 C44-F15A \\sim C44-F13
 with sigma of 0.02
 C44-F14A \\sim C44-F15
 with sigma of 0.02
 C22-F2A \\sim C22-F2
 with sigma of 0.02
 C22-F3 \\sim C22-F3A
 with sigma of 0.02
 C47-F18A \\sim C47-F16
 with sigma of 0.02
 C22-F1 \\sim C22-F1A
 with sigma of 0.02
 C47-F17A \\sim C47-F18
 with sigma of 0.02
 C47-F16A \\sim C47-F17
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C10) = Uanis(C10A)
Uanis(C12) = Uanis(C12A)
5. Others
 Sof(C10A)=Sof(H10C)=Sof(H10D)=Sof(C12A)=Sof(H12C)=Sof(H12D)=Sof(C11A)=1-FVAR(1)
 Sof(C10)=Sof(H10B)=Sof(H10A)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C11)=Sof(H11)=
 FVAR(1)
 Sof(F7A)=Sof(F8A)=Sof(F9A)=1-FVAR(2)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(2)
 Sof(F13)=Sof(F14)=Sof(F15)=1-FVAR(3)
 Sof(F13A)=Sof(F14A)=Sof(F15A)=FVAR(3)
 Sof(F16)=Sof(F17)=Sof(F18)=1-FVAR(4)
 Sof(F16A)=Sof(F17A)=Sof(F18A)=FVAR(4)
 Sof(F1A)=Sof(F2)=Sof(F3A)=1-FVAR(5)
 Sof(F1)=Sof(F2A)=Sof(F3)=FVAR(5)
6.a Ternary CH refined with riding coordinates:
 C11(H11)
6.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C3(H3), C4(H4), C7(H7), C9(H9), C15(H15), C16(H16), C17(H17),
 C20(H20), C23(H23), C26(H26), C28(H28), C31(H31), C34(H34), C37(H37), C38(H38),
  C39(H39), C42(H42), C45(H45), C48(H48), C50(H50), C53(H53), C56(H56)
6.c X=CH2 refined with riding coordinates:
 C10(H10B,H10A), C10A(H10C,H10D), C12(H12A,H12B), C12A(H12C,H12D)
6.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C)
;
_shelx_res_checksum              57700
_shelx_hkl_checksum              98586
_shelx_fab_checksum              2634
_olex2_submission_special_instructions 'No special instructions were received'