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_7042778
_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         'C24 H54 Co N3 P Si2'
_chemical_formula_sum            'C24 H54 Co N3 P Si2'
_chemical_formula_weight         530.79
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     direct
_audit_creation_date             2016-12-12
_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                81.580(2)
_cell_angle_beta                 84.062(2)
_cell_angle_gamma                80.956(2)
_cell_formula_units_Z            2
_cell_length_a                   10.9373(5)
_cell_length_b                   11.4001(5)
_cell_length_c                   12.5228(6)
_cell_measurement_reflns_used    9997
_cell_measurement_temperature    90
_cell_measurement_theta_max      31.16
_cell_measurement_theta_min      2.61
_cell_volume                     1520.21(12)
_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 0.9947
_diffrn_measured_fraction_theta_max 0.9947
_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  0.0549
_diffrn_reflns_av_unetI/netI     0.0537
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            40788
_diffrn_reflns_theta_full        31.3032
_diffrn_reflns_theta_max         31.30
_diffrn_reflns_theta_min         2.29
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.712
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6784
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1302 before and 0.0555 after correction.
The Ratio of minimum to maximum transmission is 0.9091.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.1595
_exptl_crystal_description       block
_exptl_crystal_F_000             579.3516
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.5882
_refine_diff_density_min         -0.4746
_refine_diff_density_rms         0.1130
_refine_ls_d_res_high            0.6840
_refine_ls_d_res_low             8.8849
_refine_ls_goodness_of_fit_ref   1.0251
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    76
_refine_ls_number_parameters     291
_refine_ls_number_reflns         9904
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0251
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0349P)^2^+0.3397P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0881
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                7749
_reflns_number_total             9904
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7dt00930e2.cif
_cod_data_source_block           mf1354
_cod_database_code               7042778
_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)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5a,H5b), C2(H2a,H2b), C8(H8a,H8b), C4(H4a,H4b), C6(H6a,H6b), C21(H21a,
 H21b), C9(H9a,H9b), C10(H10a,H10b)
2.c Idealised Me refined as rotating group:
 C19(H19a,H19b,H19c), C20(H20a,H20b,H20c), C18(H18a,H18b,H18c), C16(H16a,H16b,
 H16c), C3(H3a,H3b,H3c), C17(H17a,H17b,H17c), C13(H13a,H13b,H13c), C1(H1a,H1b,
 H1c), C14(H14a,H14b,H14c), C23(H23a,H23b,H23c), C24(H24a,H24b,H24c), C22(H22a,
 H22b,H22c)
;
_olex2_submission_special_instructions 'No special instructions were received'