Photoreductive chlorine elimination from a Ni(iii)Cl<sub>2</sub> complex supported by a tetradentate pyridinophane ligand.
Na, Hanah; Watson, Michael B.; Tang, Fengzhi; Rath, Nigam P.; Mirica, Liviu M.; Chemical communications (Cambridge, England) 57 (2021) 7264–7267; doi:10.1039/d1cc02114a

data_7128550
_publ_section_title
;
 Photoreductive chlorine elimination from a Ni(iii)Cl<sub>2</sub> complex
 supported by a tetradentate pyridinophane ligand.
;
_journal_issue                   59
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              7264
_journal_page_last               7267
_journal_paper_doi               10.1039/d1cc02114a
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C17 H24 Cl N4 Ni O, C H Cl3, F6 P'
_chemical_formula_sum            'C18 H25 Cl4 F6 N4 Ni O P'
_chemical_formula_weight         658.90
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-01-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-04-08 deposited with the CCDC.	2021-06-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.4628(6)
_cell_length_b                   13.3212(4)
_cell_length_c                   9.6192(3)
_cell_measurement_reflns_used    30469
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.467
_cell_measurement_theta_min      2.592
_cell_volume                     2493.95(13)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            47334
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.489
_diffrn_reflns_theta_min         2.592
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.337
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5976
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1430 before and 0.0567 after correction.
The Ratio of minimum to maximum transmission is 0.8015.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_description       needle
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.676
_exptl_crystal_size_mid          0.159
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.698
_refine_diff_density_min         -1.291
_refine_diff_density_rms         0.123
_refine_ls_abs_structure_details
;
 Flack x determined using 2592 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.015(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         5725
_refine_ls_number_restraints     140
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0316
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1040
_reflns_Friedel_coverage         0.888
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5629
_reflns_number_total             5725
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc02114a2.cif
_cod_data_source_block           33_a
_cod_depositor_comments
'Adding full bibliography for 7128549--7128550.cif.'
_cod_database_code               7128550
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.465
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O1-H1
 0.87 with sigma of 0.01
 Ni1-H1
 2.655653 with sigma of 0.02
 C17-H1
 1.882317 with sigma of 0.02
 F6-F2 \\sim F6-F4 \\sim F2-F5 \\sim F5-F4 \\sim F6A-F2A \\sim F6A-F4A \\sim
F2A-F5A \\sim F5A-F4A
 with sigma of 0.04
 P1-F1 \\sim P1-F3 \\sim P1-F6 \\sim P1-F2 \\sim P1-F5 \\sim P1-F4 \\sim P1-F6A
\\sim P1-F2A \\sim P1-F5A \\sim P1-
 F4A
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 F6, F5, F4, F2, F3, F1, P1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F6A, F4A, F2A, F1, F3, F5A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(F6A)=Sof(F2A)=Sof(F5A)=Sof(F4A)=1-FVAR(1)
 Sof(F6)=Sof(F2)=Sof(F5)=Sof(F4)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C18(H18)
5.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C7(H7A,H7B), C6(H6A,H6B), C14(H14A,H14B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C9(H9), C11(H11), C3(H3), C10(H10), C4(H4)
5.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              97934
_shelx_hkl_checksum              17856
_olex2_submission_special_instructions 'No special instructions were received'