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_7042782
_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         'C29 H51 Li N3 P'
_chemical_formula_sum            'C29 H51 Li N3 P'
_chemical_formula_weight         479.63
_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             2016-11-09
_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                 95.626(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8468(9)
_cell_length_b                   13.3188(9)
_cell_length_c                   15.9724(11)
_cell_measurement_reflns_used    9912
_cell_measurement_temperature    90
_cell_measurement_theta_max      33.86
_cell_measurement_theta_min      2.56
_cell_volume                     2931.5(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_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_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  0.0383
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            85130
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         34.080
_diffrn_reflns_theta_min         1.995
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.7234
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0853 before and 0.0485 after correction.
The Ratio of minimum to maximum transmission is 0.9688.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.087
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.34
_refine_diff_density_max         1.031
_refine_diff_density_min         -0.895
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         11949
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0568
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0811P)^2^+1.7853P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1541
_refine_ls_wR_factor_ref         0.1747
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9001
_reflns_number_total             11949
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00930e2.cif
_cod_data_source_block           mf1344
_cod_database_code               7042782
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.945
_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: H6BC(0.5) H6BD(0.5) H6AA(0.5) H6AB(0.5) C31(0.5) H31A(0.5)
 H31B(0.5) C4(0.5) H4A(0.5) H4B(0.5) C2(0.5) H2A(0.5) H2B(0.5) C3(0.5) H3A(0.5)
 H3B(0.5) H3C(0.5) C1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) C0AA(0.5) H0AA(0.5)
 H0AB(0.5) C32(0.5) H32A(0.5) H32B(0.5) C34(0.5) H34A(0.5) H34B(0.5) C33(0.5)
 H33A(0.5) H33B(0.5) H33C(0.5) C36(0.5) H36A(0.5) H36B(0.5) H36C(0.5)
3.a Ternary CH refined with riding coordinates:
 C12(H12), C24(H24), C15(H15), C27(H27)
3.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C10(H10A,H10B), C6(H6BC,H6BD), C6(H6AA,H6AB), C9(H9A,H9B),
 C31(H31A,H31B), C4(H4A,H4B), C2(H2A,H2B), C0AA(H0AA,H0AB), C32(H32A,H32B),
 C34(H34A,H34B)
3.c Aromatic/amide H refined with riding coordinates:
 C22(H22), C21(H21), C20(H20)
3.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C17(H17A,H17B,H17C), C14(H14A,H14B,H14C), C16(H16A,H16B,
 H16C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C3(H3A,H3B,H3C), C1(H1A,H1B,H1C), C33(H33A,H33B,H33C), C36(H36A,
 H36B,H36C)
;
_olex2_submission_special_instructions 'No special instructions were received'