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_7042787
_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         'C40 H86 Co N6 P2 Si2'
_chemical_formula_sum            'C40 H86 Co N6 P2 Si2'
_chemical_formula_weight         828.19
_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
_audit_creation_date             2017-01-20
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-01-20 deposited with the CCDC.
2017-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.5240(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.6761(9)
_cell_length_b                   10.0679(4)
_cell_length_c                   25.3409(12)
_cell_measurement_reflns_used    9867
_cell_measurement_temperature    90
_cell_measurement_theta_max      39.49
_cell_measurement_theta_min      2.99
_cell_volume                     4734.0(4)
_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      90.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Brulker Apex DUO'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0740
_diffrn_reflns_av_unetI/netI     0.0750
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            113854
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         39.567
_diffrn_reflns_theta_min         1.097
_exptl_absorpt_coefficient_mu    0.514
_exptl_absorpt_correction_T_max  0.7478
_exptl_absorpt_correction_T_min  0.6730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0617 before and 0.0568 after correction.
The Ratio of minimum to maximum transmission is 0.9000.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'greenish blue'
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_description       block
_exptl_crystal_F_000             1812
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.740
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         28474
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0481P)^2^+0.2109P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1133
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19178
_reflns_number_total             28474
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00930e2.cif
_cod_data_source_block           mf1338
_cod_database_code               7042787
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.865
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H28C(0.7) H28D(0.7) H28A(0.3) H28B(0.3) H31C(0.7) H31D(0.7)
 H31A(0.3) H31B(0.3) C30(0.7) H30A(0.7) H30B(0.7) C29(0.3) H29A(0.3) H29B(0.3)
3.a Ternary CH refined with riding coordinates:
 C15(H15), C33(H33), C36(H36), C12(H12)
3.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C26(H26A,H26B), C10(H10A,H10B), C24(H24A,H24B), C25(H25A,H25B),
 C6(H6A,H6B), C8(H8A,H8B), C22(H22A,H22B), C28(H28C,H28D), C28(H28A,H28B),
 C4(H4A,H4B), C5(H5A,H5B), C2(H2A,H2B), C31(H31C,H31D), C31(H31A,H31B),
 C30(H30A,H30B), C29(H29A,H29B)
3.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C39(H39A,H39B,H39C), C18(H18A,H18B,
 H18C), C20(H20A,H20B,H20C), C41(H41A,H41B,H41C), C19(H19A,H19B,H19C), C37(H37A,
 H37B,H37C), C14(H14A,H14B,H14C), C23(H23A,H23B,H23C), C38(H38A,H38B,H38C),
 C3(H3A,H3B,H3C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C21(H21A,H21B,H21C),
  C40(H40A,H40B,H40C), C13(H13A,H13B,H13C), C1(H1A,H1B,H1C)
;
_olex2_submission_special_instructions 'No special instructions were received'