Metal-metal multiple bonds in early/late heterobimetallics support unusual trigonal monopyramidal geometries at both Zr and Co.
Greenwood, Bennett P.; Rowe, Gerard T.; Chen, Chun-Hsing; Foxman, Bruce M.; Thomas, Christine M.; Journal of the American Chemical Society 132 (2010) 44–45; doi:10.1021/ja909310t

data_4101641
_publ_section_title
;
 Metal-metal multiple bonds in early/late heterobimetallics support
 unusual trigonal monopyramidal geometries at both Zr and Co.
;
_journal_issue                   1
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              44
_journal_page_last               45
_journal_paper_doi               10.1021/ja909310t
_journal_volume                  132
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C27 H63 Co1 N5 P3 Zr1'
_chemical_formula_sum            'C27 H63 Co N5 P3 Zr'
_chemical_formula_weight         700.91
_space_group_IT_number           158
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 3 -2"c'
_symmetry_space_group_name_H-M   'P 3 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             09-12-01
_audit_creation_method           CRYSTALS_ver_12.87
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   18.2757(6)
_cell_length_b                   18.2757(6)
_cell_length_c                   18.1771(6)
_cell_measurement_reflns_used    8026
_cell_measurement_temperature    120
_cell_measurement_theta_max      26
_cell_measurement_theta_min      3
_cell_volume                     5257.8(3)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Bruker Kappa Apex2'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.078
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            65308
_diffrn_reflns_theta_full        30.001
_diffrn_reflns_theta_max         30.001
_diffrn_reflns_theta_min         1.287
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.931
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2232.000
_exptl_crystal_size_max          0.127
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.120
_refine_diff_density_max         2.10
_refine_diff_density_min         -1.96
_refine_ls_abs_structure_details 'Flack (1983), 0 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.131(17)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0000
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         10237
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.0096076
_refine_ls_shift/su_mean         0.0023980
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 2.42P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0915
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0915
_reflns_limit_h_max              0
_reflns_limit_h_min              -22
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              -25
_reflns_number_gt                6277
_reflns_number_total             10237
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.75
_oxford_diffrn_Wilson_scale      255.84
_oxford_refine_ls_r_factor_ref   0.0771
_oxford_refine_ls_scale          0.054716(5)
_oxford_reflns_number_all        10237
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'BGI_119_0m in P-3c1'
_cod_data_source_file            ja909310t_si_002.cif
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      'P 3 c 1 '
_cod_original_formula_sum        'C27 H63 Co1 N5 P3 Zr1'
_cod_database_code               4101641