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_4101640
_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         'C53 H93 Co1 N5 O2 P3 Zr1'
_chemical_formula_sum            'C53 H93 Co N5 O2 P3 Zr'
_chemical_formula_weight         1075.43
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P -2ac -2n'
_symmetry_space_group_name_H-M   'P n 21 a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             09-07-15
_audit_creation_method           CRYSTALS_ver_12.87
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.3571(5)
_cell_length_b                   23.4069(5)
_cell_length_c                   21.3354(4)
_cell_measurement_reflns_used    9954
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     11165.0(4)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.062
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            198430
_diffrn_reflns_theta_full        30.085
_diffrn_reflns_theta_max         30.085
_diffrn_reflns_theta_min         1.291
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.612
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4592
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.294
_exptl_crystal_size_min          0.138
_refine_diff_density_max         1.28
_refine_diff_density_min         -1.17
_refine_ls_abs_structure_details 'Flack (1983), 0 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.313(16)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9614
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1172
_refine_ls_number_reflns         32296
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.0166749
_refine_ls_shift/su_mean         1.4754776
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 4.50 6.77 3.20 0.761 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1114
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.1114
_reflns_limit_h_max              31
_reflns_limit_h_min              0
_reflns_limit_k_max              33
_reflns_limit_k_min              -32
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                21902
_reflns_number_total             32296
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.60
_oxford_diffrn_Wilson_scale      932.57
_oxford_refine_ls_r_factor_ref   0.0726
_oxford_refine_ls_scale          0.0342937(16)
_oxford_reflns_number_all        32296
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'CMT_15_0ma in Pnma'
_cod_data_source_file            ja909310t_si_002.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1673 2011-04-08 12:14:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P n 21 a '
_cod_original_formula_sum        'C53 H93 Co1 N5 O2 P3 Zr1'
_cod_database_code               4101640