Evaluation of the coordination preferences and catalytic pathways of heteroaxial cobalt oximes towards hydrogen generation
Basu, Debashis; Mazumder, Shivnath; Niklas, Jens; Baydoun, Habib; Wanniarachchi, Dakshika; Shi, Xuetao; Staples, Richard J.; Poluektov, Oleg; Schlegel, H. Bernhard; Verani, Cláudio N.; Chem. Sci. 7 (2016) 3264–; doi:10.1039/C5SC04214C

data_1542356
_publ_section_title
;
 Evaluation of the coordination preferences and catalytic pathways of
 heteroaxial cobalt oximes towards hydrogen generation
;
_journal_issue                   5
_journal_name_full               'Chem. Sci.'
_journal_page_first              3264
_journal_paper_doi               10.1039/C5SC04214C
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C20 H30 Co N5 O2'
_chemical_formula_sum            'C20 H30 Co N5 O2'
_chemical_formula_weight         431.42
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-01-20
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-01-21 deposited with the CCDC.
2016-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.286(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.9757(13)
_cell_length_b                   10.6987(13)
_cell_length_c                   24.941(3)
_cell_measurement_reflns_used    812
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      17.06
_cell_measurement_theta_min      2.42
_cell_volume                     3954.3(8)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.1
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2264
_diffrn_reflns_av_unetI/netI     0.1783
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            24373
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.106
_diffrn_reflns_theta_max         24.106
_diffrn_reflns_theta_min         1.650
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.895
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5945
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0893 before and 0.0676 after correction.
The Ratio of minimum to maximum transmission is 0.7968.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'dark blue'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3161
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.944
_refine_ls_R_factor_all          0.1531
_refine_ls_R_factor_gt           0.0597
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0220P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0873
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1671
_reflns_number_total             3161
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc04214c2.cif
_cod_data_source_block           final4
_cod_depositor_comments
'Adding full bibliography for 1542354--1542357.cif.'
_cod_original_cell_volume        3954.3(7)
_cod_database_code               1542356
_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:
 C7(H7A,H7B), C6(H6A,H6B), C8(H8A,H8B), C4(H4A,H4B), C5(H5A,H5B)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C16(H16), C13(H13), C15(H15)
2.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C1(H1A,H1B,H1C), C18(H18A,H18B,H18C), C20(H20A,H20B,
 H20C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              57883
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'