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_7112910
_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         'C45 H75 Co1 I2 N3 P3 Zr1'
_chemical_formula_sum            'C45 H75 Co I2 N3 P3 Zr'
_chemical_formula_weight         1154.99
_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
_audit_creation_date             09-12-18
_audit_creation_method           CRYSTALS_ver_14.01
_cell_angle_alpha                90
_cell_angle_beta                 127.715(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.2429(12)
_cell_length_b                   31.7135(14)
_cell_length_c                   16.8195(7)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2
_cell_volume                     11495.3(9)
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.038
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            16791
_diffrn_reflns_theta_full        30.036
_diffrn_reflns_theta_max         30.036
_diffrn_reflns_theta_min         1.142
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.656
_exptl_absorpt_correction_T_max  0.77
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Analytical Absorption (De Meulenaer & Tompa, 1965)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'acicular fragment'
_exptl_crystal_F_000             4672
_exptl_crystal_size_max          0.473
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.160
_platon_squeeze_details
;During the structure solution, electron density difference
maps revealed that there were considerable disordered
solvent molecules (from history, likely pentane) in a
volume of 2562.8 \%A3 per unit cell (22.3%); the peaks
could not be modeled successfully. Areas of continuous
electron density appeared in the ac plane (in the
n-glide planes), creating bilayer arrangements at
b = 1/4 and 3/4.Attempts at modeling the disordered
pentane using 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.
PLATON reported a total electron density of 536 e- per
unit cell, likely representing twelve pentane molecules.
Use of the SQUEEZE technique resulted in a decrease of
ca. 1.6 % in R.
;
_refine_diff_density_max         0.92
_refine_diff_density_min         -0.66
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0639
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         16791
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0228
_refine_ls_shift/su_max          0.0050614
_refine_ls_shift/su_mean         0.0001011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.02P)^2^ +18.68P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0608
_refine_ls_wR_factor_gt          0.0515
_refine_ls_wR_factor_ref         0.0608
_reflns_limit_h_max              30
_reflns_limit_h_min              -38
_reflns_limit_k_max              44
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                13736
_reflns_number_total             16791
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.51
_oxford_diffrn_Wilson_scale      67.75
_oxford_refine_ls_r_factor_ref   0.0315
_oxford_refine_ls_scale          0.0224655(5)
_oxford_reflns_number_all        16791
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'cmt32_0m in C2/c'
_cod_data_source_file            c0cc01272f.txt
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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      'C 1 2/c 1 '
_cod_original_formula_sum        'C45 H75 Co1 I2 N3 P3 Zr1'
_cod_database_code               7112910