Phosphine-assisted C‒H bond activation in Schiff bases and formation of novel organo cobalt complexes bearing Schiff base ligands
Zhang, Hua; Xing, Junyang; Dong, Yanhong; Xie, Shangqing; Ren, Shishuai; Qi, Xinghao; Sun, Hongjian; Li, Xiaoyan; Fuhr, Olaf; Fenske, Dieter; New Journal of Chemistry 42 (2018) 4646–; doi:10.1039/C7NJ03480F

data_7056993
_publ_section_title
;
 Phosphine-assisted C--H bond activation in Schiff bases and formation of
 novel organo cobalt complexes bearing Schiff base ligands
;
_journal_issue                   6
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              4646
_journal_paper_doi               10.1039/C7NJ03480F
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C34 H30 Co N O2 P2'
_chemical_formula_sum            'C34 H30 Co N O2 P2'
_chemical_formula_weight         605.50
_chemical_name_systematic        2017Li01
_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_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-02-24
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-02-24 deposited with the CCDC.
2018-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.414(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.289(2)
_cell_length_b                   15.896(3)
_cell_length_c                   18.982(4)
_cell_measurement_reflns_used    2349
_cell_measurement_temperature    297
_cell_measurement_theta_max      23.066
_cell_measurement_theta_min      2.216
_cell_volume                     3006.9(10)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.9938
_diffrn_measured_fraction_theta_max 0.9938
_diffrn_measurement_device_type  'CCD Area Detector'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.71
_diffrn_reflns_av_R_equivalents  0.0699
_diffrn_reflns_av_unetI/netI     0.0913
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21174
_diffrn_reflns_theta_full        27.5042
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    0.706
_exptl_absorpt_correction_T_max  0.9113
_exptl_absorpt_correction_T_min  .7329
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            'metallic light yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.3376
_exptl_crystal_description       block
_exptl_crystal_F_000             1258.6669
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.8024
_refine_diff_density_min         -0.6804
_refine_diff_density_rms         0.1729
_refine_ls_d_res_high            0.7687
_refine_ls_d_res_low             12.0242
_refine_ls_goodness_of_fit_ref   1.0430
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    54
_refine_ls_number_parameters     363
_refine_ls_number_reflns         6896
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0430
_refine_ls_R_factor_all          0.1045
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0304P)^2^+0.9919P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.1048
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -13
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                4257
_reflns_number_total             6896
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7nj03480f2.cif
_cod_data_source_block           170213f_0m
_cod_depositor_comments
;

2018-03-04
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel

 Adding full bibliography for 7056990--7056993.cif.
;
_cod_original_cell_volume        3006.6(10)
_cod_original_formula_moiety     '4(C34 H30 Co N O2 P2)'
_cod_original_formula_sum        'C136 H120 Co4 N4 O8 P8'
_cod_original_formula_units_Z    1
_cod_original_formula_weight     2422.01
_cod_database_code               7056993
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H5(0) H5(0)
3.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C25(H25), C24(H24), C23(H23), C22(H22),
 C21(H21), C31(H31), C30(H30), C29(H29), C28(H28), C27(H27), C13(H13), C12(H12),
  C11(H11), C18(H18), C15(H15), C16(H16), C17(H17)
3.b Idealised Me refined as rotating group:
 C32(H32a,H32b,H32c), C33(H33a,H33b,H33c), C34(H34a,H34b,H34c)
;
_olex2_submission_original_sample_id 2017Li01
_olex2_submission_special_instructions 'No special instructions were received'