Electrocatalytic reduction of CO2 with CCC-NHC pincer nickel complexes
Cope, James D.; Liyanage, Nalaka P.; Kelley, Paul J.; Denny, Jason A.; Valente, Edward J.; Webster, Charles Edwin; Delcamp, Jared H.; Hollis, T. Keith; Chem. Commun.  (2017) –; doi:10.1039/C6CC06537F

data_7120525
_publ_section_title
;
 Electrocatalytic reduction of CO2 with CCC-NHC pincer nickel complexes
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C6CC06537F
_journal_year                    2017
_chemical_absolute_configuration unk
_chemical_formula_sum            'C20 H25 Cl N4 Ni'
_chemical_formula_weight         415.6
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-07-25T09:04:55-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2016-07-25 deposited with the CCDC.
2017-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2091(12)
_cell_length_b                   11.2996(5)
_cell_length_c                   16.6840(4)
_cell_measurement_reflns_used    10894
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      32.2039
_cell_measurement_theta_min      3.5916
_cell_volume                     1924.6(2)
_computing_cell_refinement       'CrysAlis (Oxford Diffraction)'
_computing_data_collection       'CrysAlis (Oxford Diffraction)'
_computing_data_reduction        'CrysAlis (Oxford Diffraction)'
_computing_molecular_graphics    WinGX
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 16.0309
_diffrn_detector_type            'Oxford Diffraction Sapphire 3 CCD'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_orient_matrix_UB_11      0.0500195161
_diffrn_orient_matrix_UB_12      0.0432296195
_diffrn_orient_matrix_UB_13      0.0025981057
_diffrn_orient_matrix_UB_21      0.0185138595
_diffrn_orient_matrix_UB_22      -0.0122892875
_diffrn_orient_matrix_UB_23      -0.0400125978
_diffrn_orient_matrix_UB_31      -0.0443001053
_diffrn_orient_matrix_UB_32      0.0436445302
_diffrn_orient_matrix_UB_33      -0.013833575
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23494
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.364
_diffrn_reflns_theta_min         3.606
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        <2%
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.158
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.91368
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis (Oxford Diffraction)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 1767 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
 Disorder in one of the butyl side chains modelled in SHELX, 
 and refines satisfactorily to 0.576(1) for major conformer. 
;
_refine_ls_abs_structure_Flack   0.001(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.908
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         6426
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.908
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.031
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0428P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0686
_refine_ls_wR_factor_ref         0.071
_reflns_Friedel_coverage         0.75
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.908
_reflns_number_gt                4820
_reflns_number_total             6426
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc06537f2.cif
_cod_data_source_block           up046
_cod_database_code               7120525