Formation of PCP pincer cobalt complexes with cobaltacyclopropane moieties via double Csp3-H bond activation†
zhu, gengyu; wang, lin; Sun, Hongjian; Li, Xiaoyan; RSC Adv.  (2015) –; doi:10.1039/C5RA01230A

data_7219524
_publ_section_title
;
 Formation of PCP pincer cobalt complexes with cobaltacyclopropane
 moieties via double Csp3-H bond activation&#x2020;
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA01230A
_journal_year                    2015
_chemical_formula_moiety         'C38 H40 Co N2 P3'
_chemical_formula_sum            'C38 H40 Co N2 P3'
_chemical_formula_weight         676.56
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2014-03-04
_audit_creation_method
;
Olex2 1.2
(compiled 2014.02.28 svn.r2899 for OlexSys, GUI svn.r4781)
;
_audit_update_record
;
2014-10-11 deposited with the CCDC.
2015-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.593(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.890(7)
_cell_length_b                   16.894(12)
_cell_length_c                   18.714(14)
_cell_measurement_reflns_used    603
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     3373(4)
_computing_data_reduction        'SAINT v7.23A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2030
_diffrn_reflns_av_unetI/netI     0.2727
_diffrn_reflns_Laue_measured_fraction_full 0.950
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15711
_diffrn_reflns_point_group_measured_fraction_full 0.950
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.639
_exptl_absorpt_coefficient_mu    0.681
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_F_000             1416
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.905
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         5783
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.905
_refine_ls_R_factor_all          0.2233
_refine_ls_R_factor_gt           0.0765
_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^)+(0.0567P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1314
_refine_ls_wR_factor_ref         0.1855
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2085
_reflns_number_total             5783
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra01230a2.cif
_cod_data_source_block           complex3
_cod_database_code               7219524
_shelxl_version_number           2013-4
_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. Restrained distances
 C22A-C21
 1.55 with sigma of 0.01
 C21-C22
 1.55 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C22A \\sim C22: within 1.7A with sigma of 0.002 and sigma for terminal atoms of
0.08
4. Others
 Fixed Sof: H21A(0.5) H21B(0.5) C22(0.7) H22A(0.7) H22B(0.7) H22C(0.7)
 C22A(0.3) H22D(0.3) H22E(0.3) H22F(0.3)
5.a Riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B,H22C), C22A(H22D,H22E,H22F)
5.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B)
5.c Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C)
5.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15), C16(H16), C17(H17), C24(H24), C25(H25), C26(H26), C27(H27),
  C29(H29), C30(H30), C31(H31), C32(H32), C34(H34), C35(H35), C36(H36),
 C37(H37), C38(H38)
;
_shelx_res_checksum              48536
_shelx_hkl_checksum              19703
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'