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_7042893
_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_absolute_configuration unk
_chemical_formula_moiety         'C23 H25 N2 Ni O2, B F4'
_chemical_formula_sum            'C23 H25 B F4 N2 Ni O2'
_chemical_formula_weight         506.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_Int_Tables_number      9
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-01-21
_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                 104.863(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1415(8)
_cell_length_b                   21.906(2)
_cell_length_c                   11.8206(10)
_cell_measurement_reflns_used    3969
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.440
_cell_measurement_theta_min      2.1100
_cell_volume                     2287.9(4)
_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      100.0
_diffrn_measured_fraction_theta_full 0.9662
_diffrn_measured_fraction_theta_max 0.9662
_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     0.0498
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15856
_diffrn_reflns_theta_full        26.4425
_diffrn_reflns_theta_max         26.44
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.903
_exptl_absorpt_correction_T_max  0.9962
_exptl_absorpt_correction_T_min  0.9005
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'de Meulenaar 1965'
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.4702
_exptl_crystal_description       prism
_exptl_crystal_F_000             1048.7802
_exptl_crystal_preparation       n/a
_exptl_crystal_recrystallization_method
'by slow evaporation of a concentrated CH2Cl2 solution'
_exptl_crystal_size_max          0.322
_exptl_crystal_size_mid          0.198
_exptl_crystal_size_min          0.105
_refine_diff_density_max         0.5502
_refine_diff_density_min         -0.4182
_refine_diff_density_rms         0.0805
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   8.539(15)
_refine_ls_d_res_high            0.7980
_refine_ls_d_res_low             10.9528
_refine_ls_goodness_of_fit_ref   1.0362
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    61
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4550
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.0232
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.0035
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0780P)^2^+9.5400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1373
_refine_ls_wR_factor_ref         0.1453
_reflns_Friedel_coverage         0.941
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              27
_reflns_limit_k_min              -27
_reflns_limit_l_max              14
_reflns_limit_l_min              -14
_reflns_number_gt                3969
_reflns_number_total             4550
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7dt00960g2.cif
_cod_data_source_block           ac354
_cod_original_sg_symbol_Hall     ' C -2yc'
_cod_database_code               7042893
_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(C10) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C17b) \\sim Ueq, Uanis(C18b) \\sim Ueq, Uanis(C19b) \\sim Ueq,
Uanis(C20b) \\sim Ueq, Uanis(C21b) \\sim Ueq, Uanis(C22b) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(N2b) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N2a) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(N2b) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2b) \\sim Ueq, Uanis(C24) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
: with sigma of 0.02 and sigma for terminal atoms of 0.04
: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C24a) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N2a) = Uanis(N2b)
3. Others
 Sof(O2b)=Sof(N2b)=Sof(C17b)=Sof(C18b)=Sof(C19b)=Sof(H19b)=Sof(C20b)=Sof(H20b)=
 Sof(C21b)=Sof(H21b)=Sof(C22b)=Sof(C24)=Sof(H24a)=Sof(H24b)=Sof(H24c)=Sof(H18b)=
 1-FVAR(1)
 Sof(O2a)=Sof(N2a)=Sof(C17a)=Sof(C22a)=Sof(C21a)=Sof(H21a)=Sof(C20a)=Sof(H20a)=
 Sof(C19a)=Sof(H19a)=Sof(C18a)=Sof(H18a)=FVAR(1)
 Sof(C0ab)=1-FVAR(2)
 Sof(C24a)=Sof(H24d)=Sof(H24e)=Sof(H24f)=FVAR(2)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C14(H14), C13(H13), C12(H12),
 C11(H11), C21a(H21a), C20a(H20a), C19a(H19a), C18a(H18a), C19b(H19b),
 C20b(H20b), C21b(H21b), C18b(H18b)
4.b Fitted pentagon refined as free rotating group:
 C1(C2,C3,C4,C5)
4.c Fitted hexagon refined as free rotating group:
 C10(C15,C14,C13,C12,C11), C17a(C22a,C21a,C20a,C19a,C18a), C17b(C18b,C19b,C20b,
 C21b,C22b)
4.d Idealised Me refined as rotating group:
 C6(H6a,H6b,H6c), C9(H9a,H9b,H9c), C16(H16a,H16b,H16c), C24(H24c,H24b,H24a),
 C24a(H24d,H24e,H24f)
;
_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'