A pentadentate nitrogen-rich copper electrocatalyst for water reduction with pH-dependent molecular mechanisms
Ekanayake, Danushka M.; Kulesa, Krista M.; Singh, Jaffarguriqbal; Kpogo, Kenneth Kwame; Mazumder, Shivnath; Schlegel, H. Bernhard; Verani, Claudio; Dalton Trans.  (2017) –; doi:10.1039/C7DT02711G

data_7044063
_publ_section_title
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 A pentadentate nitrogen-rich copper electrocatalyst for water reduction
 with pH-dependent molecular mechanisms
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02711G
_journal_year                    2017
_chemical_formula_moiety         'C25 H25 Cu N5, F6 P'
_chemical_formula_sum            'C25 H25 Cu F6 N5 P'
_chemical_formula_weight         604.02
_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_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-09
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-07-21 deposited with the CCDC.
2017-08-31 downloaded from the CCDC.
;
_cell_angle_alpha                93.317(3)
_cell_angle_beta                 91.601(3)
_cell_angle_gamma                99.641(3)
_cell_formula_units_Z            4
_cell_length_a                   9.9304(5)
_cell_length_b                   15.6402(8)
_cell_length_c                   16.5800(8)
_cell_measurement_reflns_used    9956
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.62
_cell_measurement_theta_min      2.55
_cell_volume                     2532.6(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100.1
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.9921
_diffrn_measured_fraction_theta_max 0.9921
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0629
_diffrn_reflns_av_unetI/netI     0.0501
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            56125
_diffrn_reflns_theta_full        25.3449
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         1.23
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.995
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.6658
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0800 before and 0.0585 after correction.
The Ratio of minimum to maximum transmission is 0.8912.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.5840
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1234.4362
_exptl_crystal_size_max          1.15
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.5949
_refine_diff_density_min         -0.5505
_refine_diff_density_rms         0.1184
_refine_ls_d_res_high            0.8302
_refine_ls_d_res_low             16.5401
_refine_ls_goodness_of_fit_ref   1.0368
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    90
_refine_ls_number_parameters     686
_refine_ls_number_reflns         9182
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0368
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0235P)^2^+2.1556P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0760
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              18
_reflns_limit_k_min              -18
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                6959
_reflns_number_total             9182
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7dt02711g2.cif
_cod_data_source_block           final1
_cod_depositor_comments
;

2017-11-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C25 H25 Cu N5), 2(F6 P)'
_cod_original_formula_sum        'C50 H50 Cu2 F12 N10 P2'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1208.04
_cod_database_code               7044063
_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:
 C10(H10a,H10b), C2(H2a,H2b), C6(H6a,H6b), C11(H11a,H11b), C31(H31a,H31b),
 C43(H43a,H43b)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C9(H9), C0AA(H0AA), C13(H13), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24),
  C26(H26), C27(H27), C28(H28), C29(H29), C33(H33), C34(H34), C35(H35),
 C36(H36), C39(H39), C40(H40), C41(H41), C42(H42), C45(H45), C46(H46), C47(H47),
  C48(H48)
2.c Idealised Me refined as rotating group:
 C3(H3a,H3b,H3c), C37(H37a,H37b,H37c)
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_olex2_submission_special_instructions 'No special instructions were received'