Peripheral Methyl Activation in η4-1,2,3,4-Tetramethylcyclobutadienylcobalt Complexes: Template Synthesis and Subsequent Reactivity of Triphosphamacrocycles
Edwards, Peter G.; Kariuki, Benson M.; Newman, Paul D.; Zhang, Wenjian; Organometallics 33 (2014) 5440–; doi:10.1021/om500734b

data_4084338
_publ_section_title
;
 Peripheral Methyl Activation in
 \h4-1,2,3,4-Tetramethylcyclobutadienylcobalt Complexes: Template
 Synthesis and Subsequent Reactivity of Triphosphamacrocycles
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5440
_journal_paper_doi               10.1021/om500734b
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C44 H35 Co P3, Sb F6, C2 H3 N'
_chemical_formula_sum            'C46 H38 Co F6 N P3 Sb'
_chemical_formula_weight         992.36
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.8180(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.7573(5)
_cell_length_b                   14.1366(2)
_cell_length_c                   19.5726(4)
_cell_measurement_reflns_used    6649
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      3.41
_cell_volume                     8175.3(2)
_computing_cell_refinement       DENZO/SCALEPACK
_computing_data_collection       'cOLLECT,Nonius BV, 1997-2001'
_computing_data_reduction        DENZO/SCALEPACK
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SHELXs-97
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'CCD scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0001
_diffrn_reflns_av_sigmaI/netI    0.0691
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9336
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         3.41
_exptl_absorpt_coefficient_mu    1.247
_exptl_absorpt_correction_T_max  0.8855
_exptl_absorpt_correction_T_min  0.7457
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Denzo/Scalepack
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3984
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.154
_refine_diff_density_min         -1.248
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         9336
_refine_ls_number_restraints     240
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0728
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0810P)^2^+49.9929P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1729
_refine_ls_wR_factor_ref         0.1938
_reflns_number_gt                6649
_reflns_number_total             9336
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500734b_si_002.cif
_cod_data_source_block           cmpd7
_cod_depositor_comments
'Adding full bibliography for 4084333--4084338.cif.'
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4084338
_publcif_datablock.id            {ce3dc451-0107-450d-8eb6-2e6309044932}
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