Electrochemical reduction of carbon dioxide with a molecular polypyridyl nickel complex
Lieske, Lauren E.; Rheingold, Arnold L.; Machan, Charles W.; Sustainable Energy & Fuels 2 (2018) 1269–; doi:10.1039/C8SE00027A

data_1554610
_publ_section_title
;
 Electrochemical reduction of carbon dioxide with a molecular polypyridyl
 nickel complex
;
_journal_issue                   6
_journal_name_full               'Sustainable Energy &amp; Fuels'
_journal_page_first              1269
_journal_paper_doi               10.1039/C8SE00027A
_journal_volume                  2
_journal_year                    2018
_chemical_formula_moiety         'C26 H28 N6 Ni, 2(F6 P)'
_chemical_formula_sum            'C26 H28 F12 N6 Ni P2'
_chemical_formula_weight         773.19
_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             2017-08-30
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-01-15 deposited with the CCDC.
2018-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.970(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8699(6)
_cell_length_b                   17.1455(7)
_cell_length_c                   14.2982(8)
_cell_measurement_reflns_used    2343
_cell_measurement_temperature    100
_cell_measurement_theta_max      22.169
_cell_measurement_theta_min      2.565
_cell_volume                     3338.1(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'APEX2 v2013.6-2 (Bruker, 2013)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'XT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX CCD'
_diffrn_detector_area_resol_mean 8.0
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_av_unetI/netI     0.0868
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15877
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.027
_diffrn_reflns_theta_min         2.565
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.772
_exptl_absorpt_correction_T_max  0.4293
_exptl_absorpt_correction_T_min  0.3852
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0494 before and 0.0440 after correction. The Ratio of minimum to maximum transmission is 0.8973. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_description       plate
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.516
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         6314
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0384P)^2^+1.0052P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.1046
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4096
_reflns_number_total             6314
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8se00027a2.cif
_cod_data_source_block           p21n_a_sq
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               1554610
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.927
_shelx_estimated_absorpt_t_min   0.825
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C26(H26A,H26B), C19(H19A,H19B), C18(H18A,H18B),
 C25(H25A,H25B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C13(H13), C4(H4), C3(H3), C24(H24), C15(H15), C9(H9), C2(H2),
 C12(H12), C16(H16), C21(H21), C14(H14), C11(H11), C23(H23), C10(H10), C22(H22)
;
_shelx_res_checksum              21821
_shelx_hkl_checksum              78493
_shelx_fab_checksum              91611
_olex2_submission_special_instructions 'No special instructions were received'