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_1542354
_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         'C23 H28 Cl Co N5 O3, F6 P'
_chemical_formula_sum            'C23 H28 Cl Co F6 N5 O3 P'
_chemical_formula_weight         661.85
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-01-21
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_audit_update_record
;
2015-11-03 deposited with the CCDC.
2016-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 96.4950(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.9686(4)
_cell_length_b                   22.9724(13)
_cell_length_c                   17.7667(12)
_cell_measurement_reflns_used    9943
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.94
_cell_measurement_theta_min      2.31
_cell_volume                     2825.9(3)
_computing_cell_refinement       'APEX2 (BRUKER, V2012.10-0, 2012)'
_computing_data_collection       'COSMO (BRUKER, V1.61, 2009)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 836.6
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0760
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            46377
_diffrn_reflns_theta_full        25.39
_diffrn_reflns_theta_max         25.39
_diffrn_reflns_theta_min         1.45
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.833
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0660 before and 0.0578 after correction.
The Ratio of minimum to maximum transmission is 0.9328.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.162
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.039
_refine_diff_density_max         0.551
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         5201
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0518
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0940P)^2^+1.4990P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1385
_refine_ls_wR_factor_ref         0.1609
_reflns_number_gt                3752
_reflns_number_total             5201
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5sc04214c2.cif
_cod_data_source_block           cnv413
_cod_depositor_comments
'Adding full bibliography for 1542354--1542357.cif.'
_cod_database_code               1542354
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H20 of C20, H19 of C19, H16 of C16, H21 of C21, H23 of C23, H22 of C22,
  {H5A,H5B} of C5, {H7A,H7B} of C7, H15 of C15, H13 of C13, H12 of C12, {H6A,
  H6B} of C6
 At 1.5 times of:
  H1 of O1, {H8A,H8B,H8C} of C8, {H11A,H11B,H11C} of C11, {H4A,H4B,H4C} of C4,
   {H1A,H1B,H1C} of C1
2.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21),
 C22(H22), C23(H23)
2.c Tetrahedral OH refined with riding coordinates:
 O1(H1)
2.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C4(H4A,H4B,H4C), C8(H8A,H8B,H8C), C11(H11A,H11B,H11C)
;
_contact_crystallographer_email  staples@chemistry.msu.com
_contact_crystallographer_name   'Richard Staples'