Variable Coordination Geometries via an Amine-Tethered-Enamidophosphinimine Ligand on Cobalt
Suzuki, Tatsuya; Masuda, Hideki; Fryzuk, Michael D.; Dalton Trans.  (2017) –; doi:10.1039/C7DT00930E

data_7042784
_publ_section_title
;
 Variable Coordination Geometries via an
 Amine-Tethered-Enamidophosphinimine Ligand on Cobalt
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00930E
_journal_year                    2017
_chemical_formula_moiety         'C58 H104 Co2 N6 P2'
_chemical_formula_sum            'C58 H104 Co2 N6 P2'
_chemical_formula_weight         1065.33
_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_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2016-11-22
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2016-12-12 deposited with the CCDC.
2017-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 122.438(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.716(7)
_cell_length_b                   10.304(3)
_cell_length_c                   25.239(9)
_cell_measurement_reflns_used    9252
_cell_measurement_temperature    90
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.54
_cell_volume                     6083(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9972
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            52628
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         1.74
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.637
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0476 before and 0.0440 after correction.
The Ratio of minimum to maximum transmission is 0.9269.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.1632
_exptl_crystal_description       cube
_exptl_crystal_F_000             2316.2371
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.5745
_refine_diff_density_min         -0.3147
_refine_diff_density_rms         0.0619
_refine_ls_d_res_high            0.7683
_refine_ls_d_res_low             11.6958
_refine_ls_goodness_of_fit_ref   1.0502
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    75
_refine_ls_number_parameters     320
_refine_ls_number_reflns         7013
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0502
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0284
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+6.3826P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0745
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              30
_reflns_limit_h_min              -36
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              32
_reflns_limit_l_min              0
_reflns_number_gt                6192
_reflns_number_total             7013
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7dt00930e2.cif
_cod_data_source_block           mf1347
_cod_database_code               7042784
_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 Ternary CH refined with riding coordinates:
 C27(H27), C24(H24), C15(H15), C12(H12)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6a,H6b), C5(H5a,H5b), C8(H8a,H8b), C9(H9a,H9b), C10(H10a,H10b), C4(H4a,
 H4b), C2(H2a,H2b)
2.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C20(H20), C22(H22)
2.d Idealised Me refined as rotating group:
 C25(H25a,H25b,H25c), C28(H28a,H28b,H28c), C29(H29a,H29b,H29c), C17(H17a,H17b,
 H17c), C13(H13a,H13b,H13c), C16(H16a,H16b,H16c), C14(H14a,H14b,H14c), C3(H3a,
 H3b,H3c), C26(H26a,H26b,H26c), C1(H1a,H1b,H1c)
;
_olex2_submission_special_instructions 'No special instructions were received'