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_7042786
_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         'C20 H42 Co N3 P Si'
_chemical_formula_sum            'C20 H42 Co N3 P Si'
_chemical_formula_weight         442.55
_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             2016-11-24
_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                 107.622(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8978(12)
_cell_length_b                   10.1985(10)
_cell_length_c                   18.5025(18)
_cell_measurement_reflns_used    9784
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      44.17
_cell_measurement_theta_min      2.40
_cell_volume                     2319.6(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      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.977
_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  0.0555
_diffrn_reflns_av_unetI/netI     0.0545
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            72213
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         44.214
_diffrn_reflns_theta_min         2.307
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.870
_exptl_absorpt_correction_T_max  0.7487
_exptl_absorpt_correction_T_min  0.6734
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0606 before and 0.0560 after correction.
The Ratio of minimum to maximum transmission is 0.8994.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_description       block
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.641
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         17933
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0357
_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^)+(0.0341P)^2^+0.2079P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0871
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13012
_reflns_number_total             17933
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00930e2.cif
_cod_data_source_block           mf1346
_cod_database_code               7042786
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.866
_shelx_estimated_absorpt_t_min   0.799
_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:
 C6(H6a,H6b), C8(H8a,H8b), C20(H20a,H20b), C4(H4a,H4b), C5(H5a,H5b), C2(H2a,
 H2b), C10(H10a,H10b), C9(H9a,H9b)
2.c Idealised Me refined as rotating group:
 C19(H19a,H19b,H19c), C18(H18a,H18b,H18c), C1(H1a,H1b,H1c), C13(H13a,H13b,
 H13c), C14(H14a,H14b,H14c), C17(H17a,H17b,H17c), C16(H16a,H16b,H16c), C3(H3a,
 H3b,H3c)
;
_olex2_submission_special_instructions 'No special instructions were received'