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_7042785
_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 H50 Cl Co N3 P, 0.5(C4 H10 O)'
_chemical_formula_sum            'C31 H55 Cl Co N3 O0.5 P'
_chemical_formula_weight         603.12
_chemical_name_systematic
;
 ?
;
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-01-23
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-01-23 deposited with the CCDC.
2017-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                105.750(6)
_cell_angle_beta                 107.780(6)
_cell_angle_gamma                90.106(6)
_cell_formula_units_Z            4
_cell_length_a                   12.7531(15)
_cell_length_b                   15.1301(18)
_cell_length_c                   18.634(2)
_cell_measurement_reflns_used    9928
_cell_measurement_temperature    90
_cell_measurement_theta_max      25.05
_cell_measurement_theta_min      2.29
_cell_volume                     3281.1(7)
_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 0.869
_diffrn_measured_fraction_theta_max 0.963
_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  0.0484
_diffrn_reflns_av_unetI/netI     0.0605
_diffrn_reflns_Laue_measured_fraction_full 0.869
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34822
_diffrn_reflns_point_group_measured_fraction_full 0.869
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.076
_diffrn_reflns_theta_min         1.197
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.678
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0853 before and 0.0779 after correction.
 The Ratio of minimum to maximum transmission is 0.69.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 22789 reflections, Rint = 0.0549
 (9392 with I > 3sig(I), Rint = 0.0452)
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_description       plate
_exptl_crystal_F_000             1300
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         4.060
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         11225
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1090
_refine_ls_R_factor_gt           0.0885
_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^)+(0.1325P)^2^+19.7767P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2282
_refine_ls_wR_factor_ref         0.2449
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8638
_reflns_number_total             11225
_reflns_threshold_expression     'I > 2\s(I)'
_cod_depositor_comments
;

2017-10-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C62 H110 Cl2 Co2 N6 O P2'
_cod_original_formula_weight         1206.25
_cod_original_formula_moiety
'C29 H51 Cl Co N3 P, C29 H49 Cl Co N3 P, C4 H10 O'
_cod_original_formula_units_Z            2
_cod_data_source_file            c7dt00930e2.cif
_cod_data_source_block           mf1325
_cod_database_code               7042785
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.893
_shelx_estimated_absorpt_t_min   0.849
_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:
 C24(H24), C53(H53), C15(H15), C44(H44), C41(H41), C12(H12), C56(H56), C27(H27)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5a,H5b), C34(H34a,H34b), C35(H35a,H35b), C6(H6a,H6b), C31(H31a,H31b),
 C39(H39a,H39b), C33(H33a,H33b), C37(H37a,H37b), C2(H2a,H2b), C8(H8a,H8b),
 C10(H10a,H10b), C38(H38a,H38b), C9(H9a,H9b), C60(H60a,H60b), C61(H61a,H61b)
2.c Aromatic/amide H refined with riding coordinates:
 C22(H22), C50(H50), C51(H51), C49(H49), C20(H20), C21(H21)
2.d Idealised Me refined as rotating group:
 C16(H16a,H16b,H16c), C1(H1a,H1b,H1c), C30(H30a,H30b,H30c), C17(H17a,H17b,
 H17c), C42(H42a,H42b,H42c), C26(H26a,H26b,H26c), C32(H32a,H32b,H32c), C14(H14a,
 H14b,H14c), C28(H28a,H28b,H28c), C43(H43a,H43b,H43c), C3(H3a,H3b,H3c),
 C45(H45a,H45b,H45c), C25(H25a,H25b,H25c), C54(H54a,H54b,H54c), C58(H58a,H58b,
 H58c), C57(H57a,H57b,H57c), C13(H13a,H13b,H13c), C46(H46a,H46b,H46c), C55(H55a,
 H55b,H55c), C29(H29a,H29b,H29c), C62(H62a,H62b,H62c), C59(H59a,H59b,H59c)
;
_olex2_submission_special_instructions 'No special instructions were received'