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_7042779
_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         'C33 H62 Co N3 P Si'
_chemical_formula_sum            'C33 H62 Co N3 P Si'
_chemical_formula_weight         618.84
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-21
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-09-06 deposited with the CCDC.
2017-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.751(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9978(5)
_cell_length_b                   20.9247(11)
_cell_length_c                   16.7898(9)
_cell_measurement_reflns_used    9957
_cell_measurement_temperature    90
_cell_measurement_theta_max      26.43
_cell_measurement_theta_min      2.26
_cell_volume                     3504.9(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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28373
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.432
_diffrn_reflns_theta_min         1.557
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5650
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1142 before and 0.0565 after correction.
The Ratio of minimum to maximum transmission is 0.7580.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_description       prism
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.919
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         7191
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0732P)^2^+1.3030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1205
_refine_ls_wR_factor_ref         0.1284
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5907
_reflns_number_total             7191
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00930e2.cif
_cod_data_source_block           mf1308
_cod_database_code               7042779
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.885
_shelx_estimated_absorpt_t_min   0.819
_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:
 C12(H12), C15(H15), C27(H27), C24(H24)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C30(H30A,H30B), C5(H5A,H5B), C8(H8A,H8B), C6(H6A,H6B), C4(H4A,
 H4B), C10(H10A,H10B), C9(H9A,H9B)
2.c Aromatic/amide H refined with riding coordinates:
 C22(H22), C20(H20), C21(H21)
2.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C33(H33A,H33B,H33C), C13(H13A,H13B,H13C), C1(H1A,H1B,
 H1C), C29(H29A,H29B,H29C), C25(H25A,H25B,H25C), C16(H16A,H16B,H16C), C17(H17A,
 H17B,H17C), C26(H26A,H26B,H26C), C3(H3A,H3B,H3C), C31(H31A,H31B,H31C),
 C32(H32A,H32B,H32C), C28(H28A,H28B,H28C)
;
_olex2_submission_special_instructions 'No special instructions were received'