Oxidative addition across Zr/Co multiple bonds in early/late heterobimetallic complexes.
Thomas, Christine M.; Napoline, J. Wesley; Rowe, Gerard T.; Foxman, Bruce M.; Chemical communications (Cambridge, England) 46 (2010) 5790–5792; doi:10.1039/c0cc01272f

data_7112913
_publ_section_title
;
 Oxidative addition across Zr/Co multiple bonds in early/late
 heterobimetallic complexes.
;
_journal_issue                   31
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5790
_journal_page_last               5792
_journal_paper_doi               10.1039/c0cc01272f
_journal_volume                  46
_journal_year                    2010
_chemical_formula_moiety         'C50 H86 Cl0.85 Co1 I0.15 N3 P3 Zr1'
_chemical_formula_sum            'C50 H86 Cl0.85 Co I0.15 N3 P3 Zr'
_chemical_formula_weight         1021.32
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-02-15
_audit_creation_method           CRYSTALS_ver_14.01
_cell_angle_alpha                77.154(3)
_cell_angle_beta                 82.246(2)
_cell_angle_gamma                79.036(2)
_cell_formula_units_Z            2
_cell_length_a                   12.2227(5)
_cell_length_b                   14.2597(7)
_cell_length_c                   18.3302(9)
_cell_measurement_reflns_used    9908
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     3043.6(2)
_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 0.990
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_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  0.049
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            17679
_diffrn_reflns_theta_full        29.468
_diffrn_reflns_theta_max         30.070
_diffrn_reflns_theta_min         2.067
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.665
_exptl_absorpt_correction_T_max  0.81
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Analytical Absorption (De Meulenaer & Tompa, 1965)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.114
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'prism fragment'
_exptl_crystal_F_000             1082.664
_exptl_crystal_size_max          0.583
_exptl_crystal_size_mid          0.403
_exptl_crystal_size_min          0.319
_platon_squeeze_details
;
During the structure solution, electron density difference
maps revealed that there were considerable disordered
solvent molecules. One pentane molecule was located
and successfully refined. From history, the remaining
solvate was likely pentane or toluene in a volume of
588.8 \%A3 per unit cell (19.3%); the remaining peaks
could not be modeled successfully. It appeared that
the cavity area contained about two pentane molecules,
located near the center of symmetry at (0, 1/2, 0).
Modeling with or without restraints was unsuccessful,
as was step by step acquisition of peaks using successive
electron density difference maps. Thus, the structure
factors were modified using the PLATON SQUEEZE technique,
in order to produce a ?solvate-free? structure factor set
(only for the second independent pentane molecule.)
PLATON reported a total electron density of 70 e- per
unit cell, likely representing two pentane molecules,
consistent with our earlier observations. Use of the
SQUEEZE technique resulted in a decrease of ca 1.3 % in R.
;
_refine_diff_density_max         2.53
_refine_diff_density_min         -1.28
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9847
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         17679
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0669
_refine_ls_shift/su_max          0.0040489
_refine_ls_shift/su_mean         8.1273460
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.09P)^2^ +14.84P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2032
_refine_ls_wR_factor_gt          0.1773
_refine_ls_wR_factor_ref         0.2032
_reflns_limit_h_max              17
_reflns_limit_h_min              -16
_reflns_limit_k_max              20
_reflns_limit_k_min              -19
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                12534
_reflns_number_total             17679
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.95
_oxford_diffrn_Wilson_scale      163.70
_oxford_refine_ls_r_factor_ref   0.0943
_oxford_refine_ls_scale          0.13780(6)
_oxford_reflns_number_all        17679
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'CMT36_0m in P-1'
_cod_data_source_file            c0cc01272f.txt
_cod_data_source_block           7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

data name '_diffrn_measurement_device-type' was replaced with
'_diffrn_measurement_device_type' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C50 H86 Cl0.85 Co1 I0.15 N3 P3 Zr1'
_cod_database_code               7112913