Tuning the overpotential of electrocatalytically active cyclopentadienylnickel complexes containing 1,4-diaza-1,3-butadienes (DAB) for proton reduction.
Sondermann, Christina; Ringenberg, Mark R.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 5143–5146; doi:10.1039/c7dt00960g

data_7042892
_publ_section_title
;
 Tuning the overpotential of electrocatalytically active
 cyclopentadienylnickel complexes containing 1,4-diaza-1,3-butadienes
 (DAB) for proton reduction.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5143
_journal_page_last               5146
_journal_paper_doi               10.1039/c7dt00960g
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'B F4, C21 H21 N2 Ni'
_chemical_formula_sum            'C21 H21 B F4 N2 Ni'
_chemical_formula_weight         446.93
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-02-04
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-09-14 deposited with the CCDC.
2017-03-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9844(8)
_cell_length_b                   15.3276(11)
_cell_length_c                   10.8448(8)
_cell_measurement_reflns_used    1756
_cell_measurement_temperature    100
_cell_measurement_theta_max      0.745
_cell_measurement_theta_min      0.642
_cell_volume                     1992.1(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.02
_diffrn_measured_fraction_theta_full 0.9963
_diffrn_measured_fraction_theta_max 0.9963
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            24840
_diffrn_reflns_theta_full        26.4699
_diffrn_reflns_theta_max         26.47
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    1.019
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6418
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing 1995'
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.4900
_exptl_crystal_description       needle
_exptl_crystal_F_000             921.8941
_exptl_crystal_preparation       none
_exptl_crystal_recrystallization_method 'slow evaporation of CH2Cl2 solution'
_exptl_crystal_size_max          0.594
_exptl_crystal_size_mid          0.194
_exptl_crystal_size_min          0.167
_refine_diff_density_max         0.6944
_refine_diff_density_min         -0.5992
_refine_diff_density_rms         0.0775
_refine_ls_d_res_high            0.7973
_refine_ls_d_res_low             8.8530
_refine_ls_goodness_of_fit_ref   1.0667
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    20
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2133
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.0434
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0311
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1290
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              0
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                1756
_reflns_number_total             2133
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7dt00960g2.cif
_cod_data_source_block           ac353
_cod_database_code               7042892
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C2) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C3) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.01
3.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C8(H8), C11(H11), C10(H10)
3.c Idealised Me refined as rotating group:
 C5(H5a,H5b,H5c)
;
_olex2_exptl_crystal_mounting_method
'crystals were mounted using perfluoropolyalkylether from ABCR viscosity 1800 cts on to a cryoloop'
_olex2_submission_special_instructions 'No special instructions were received'