Electronic Factors Affecting Metal−Metal Interactions in Early/Late Heterobimetallics: Substituent Effects in Zirconium/Platinum Bis(phosphinoamide) Complexes†
Cooper, Benjamin G.; Fafard, Claudia M.; Foxman, Bruce M.; Thomas, Christine M.; Organometallics 29 (2010) 5179–; doi:10.1021/om100356a

data_4066211
_publ_section_title
;
 Electronic Factors Affecting Metal&#x2212;Metal Interactions in
 Early/Late Heterobimetallics: Substituent Effects in Zirconium/Platinum
 Bis(phosphinoamide) Complexes&#x2020;
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5179
_journal_paper_doi               10.1021/om100356a
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C36 H51 Cl1 N2 P2 Pt1 Si1 Zr1'
_chemical_formula_sum            'C36 H51 Cl N2 P2 Pt Si Zr'
_chemical_formula_weight         923.61
_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             09-12-06
_audit_creation_method           CRYSTALS_ver_12.87
_cell_angle_alpha                78.7040(10)
_cell_angle_beta                 84.2540(10)
_cell_angle_gamma                75.9310(10)
_cell_formula_units_Z            2
_cell_length_a                   11.0436(3)
_cell_length_b                   12.4138(3)
_cell_length_c                   18.0560(4)
_cell_measurement_reflns_used    9871
_cell_measurement_temperature    190
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     2351.00(10)
_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    'CRYSTALS (Betteridge et al., 2003)'
_diffrn_ambient_temperature      190
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.039
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13709
_diffrn_reflns_theta_full        30.008
_diffrn_reflns_theta_max         30.008
_diffrn_reflns_theta_min         1.152
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.366
_exptl_absorpt_correction_T_max  0.67
_exptl_absorpt_correction_T_min  0.56
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker AXS, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'plate fragment'
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.335
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.118
_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 568.4 A3 
per unit cell (24.2%); the peaks could not be modeled successfully.  
It appeared that the cavity area contained about three pentane 
molecules, near centers of symmetry at (0 0 1/2), (0 1/2 1/2) 
and (1/2 1/2 1/2).  Modeling 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 126 e- per unit cell, likely representing 
three 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         1.01
_refine_diff_density_min         -0.66
_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     397
_refine_ls_number_reflns         13709
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0227
_refine_ls_shift/su_max          0.0014212
_refine_ls_shift/su_mean         4.5491867
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.02P)^2^ + 1.09P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0506
_refine_ls_wR_factor_gt          0.0496
_refine_ls_wR_factor_ref         0.0506
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              17
_reflns_limit_k_min              -16
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                11695
_reflns_number_total             13709
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.82
_oxford_diffrn_Wilson_scale      197.18
_oxford_refine_ls_r_factor_ref   0.0299
_oxford_refine_ls_scale          0.105008(10)
_oxford_reflns_number_all        13709
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'BGC_18_0m in P-1'
_cod_data_source_file            om100356a_si_002.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C36 H51 Cl1 N2 P2 Pt1 Si1 Zr1'
_cod_database_code               4066211