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_4518614
_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 H60 N2 Ni O'
_chemical_formula_sum            'C59 H60 N2 Ni O'
_chemical_formula_weight         871.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                90
_cell_angle_beta                 106.372(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2781(5)
_cell_length_b                   22.6085(10)
_cell_length_c                   18.0159(7)
_cell_measurement_reflns_used    39664
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      1.80
_cell_volume                     4798.2(4)
_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 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
 360 frames, detector distance = 90 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  0.0870
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            65484
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.037
_diffrn_reflns_theta_min         1.483
_exptl_absorpt_coefficient_mu    0.447
_exptl_absorpt_correction_T_max  0.8746
_exptl_absorpt_correction_T_min  0.5575
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.367
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.392
_refine_diff_density_min         -1.065
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       0.0046(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    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         10472
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0819P)^2^+1.6502P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1450
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7421
_reflns_number_total             10472
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c00778_si_004.cif
_cod_data_source_block           esrs11
_cod_database_code               4518614
_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,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H13C)=Sof(H13D)=Sof(H15C)=Sof(H15D)=Sof(C14B)=Sof(H14B)=1-FVAR(1)
 Sof(H13A)=Sof(H13B)=Sof(H15A)=Sof(H15B)=Sof(C14A)=Sof(H14A)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C14A(H14A), C14B(H14B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C10(H10), C12(H12), C18(H18), C19(H19), C20(H20), C23(H23),
 C26(H26), C29(H29), C31(H31), C34(H34), C37(H37), C40(H40), C41(H41), C42(H42),
  C45(H45), C48(H48), C51(H51), C53(H53), C56(H56), C59(H59)
3.c X=CH2 refined with riding coordinates:
 C13(H13C,H13D), C13(H13A,H13B), C15(H15A,H15B), C15(H15C,H15D)
3.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C25(H25A,H25B,H25C),
 C28(H28A,H28B,H28C), C33(H33A,H33B,H33C), C36(H36A,H36B,H36C), C47(H47A,H47B,
 H47C), C50(H50A,H50B,H50C), C55(H55A,H55B,H55C), C58(H58A,H58B,H58C)
;
_shelx_res_checksum              82603
_shelx_hkl_checksum              95905
_olex2_submission_special_instructions 'No special instructions were received'