Synthesis and comparison of nickel, palladium, and platinum bis(N-heterocyclic carbene) pincer complexes for electrocatalytic CO<sub>2</sub> reduction.
Therrien, J. A.; Wolf, M. O.; Patrick, B. O.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 1827–1840; doi:10.1039/c7dt04089j

data_7045217
_publ_section_title
;
 Synthesis and comparison of nickel, palladium, and platinum
 bis(N-heterocyclic carbene) pincer complexes for electrocatalytic
 CO<sub>2</sub> reduction.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1827
_journal_page_last               1840
_journal_paper_doi               10.1039/c7dt04089j
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C29 H33 Cl N5 Ni, C F3 O3 S'
_chemical_formula_sum            'C30 H33 Cl F3 N5 Ni O3 S'
_chemical_formula_weight         694.83
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-02-02
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-10-27 deposited with the CCDC.
2017-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                89.824(8)
_cell_angle_beta                 89.273(8)
_cell_angle_gamma                67.244(8)
_cell_formula_units_Z            2
_cell_length_a                   10.561(3)
_cell_length_b                   10.647(3)
_cell_length_c                   14.867(4)
_cell_measurement_reflns_used    9865
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.15
_cell_measurement_theta_min      2.31
_cell_volume                     1541.4(7)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'Bruker D8 Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            39654
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.196
_diffrn_reflns_theta_min         2.074
_diffrn_source                   'sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.843
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0525 before and 0.0463 after correction.
The Ratio of minimum to maximum transmission is 0.9173.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_description       irregular
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.508
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         9056
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0325P)^2^+0.8300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0803
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7233
_reflns_number_total             9056
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04089j2.cif
_cod_data_source_block           mw265
_cod_depositor_comments          'Adding full bibliography for 7045217.cif.'
_cod_original_cell_volume        1541.4(8)
_cod_database_code               7045217
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.843
_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
2.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C12(H12A,H12B), C18(H18A,H18B),
 C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C14(H14), C15(H15), C16(H16), C21(H21),
 C22(H22), C23(H23), C24(H24)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              72598
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'