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_4066210
_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         'C40 H56 Cl2 N2 O2 P2 Pt1 Zr1'
_chemical_formula_sum            'C40 H56 Cl2 N2 O2 P2 Pt Zr'
_chemical_formula_weight         1016.06
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             09-12-12
_audit_creation_method           CRYSTALS_ver_12.87
_cell_angle_alpha                90
_cell_angle_beta                 90.455(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3496(4)
_cell_length_b                   34.5901(15)
_cell_length_c                   13.6659(5)
_cell_measurement_reflns_used    9113
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     4419.5(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 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       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12928
_diffrn_reflns_theta_full        30.042
_diffrn_reflns_theta_max         30.042
_diffrn_reflns_theta_min         1.602
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.624
_exptl_absorpt_correction_T_max  0.66
_exptl_absorpt_correction_T_min  0.37
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker AXS, 2006)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.273
_exptl_crystal_size_min          0.116
_platon_squeeze_details
;
During the structure solution, electron density difference 
maps revealed that there was a coordinated THF and two 
THF solvate molecules in the asymmetric unit.  The 
coordinated THF and one of the solvate molecules were 
successfully modeled.  The solvate THF was disordered, 
with the oxygen atom occupying two positions (O20, O21) 
whose occupancies were constrained to sum to 1.0; the 
major component had a refined occupancy of 0.85(2).  
The other THF could not be successfully modeled, and 
PLATON SQUEEZE reported two molecules (ca. 92 e-/cell) 
in a void volume of 486.8 A3 per unit cell (11.0 %).  
The electron density near centers of symmetry at 
(0 0 1/2) and (0 1/2 0).  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 SQUEEZE3,4 technique, in order to produce a 
"solvate-free" structure factor set.  Use of the 
SQUEEZE technique resulted in a decrease of ca 1 % in R.  
;
_refine_diff_density_max         0.89
_refine_diff_density_min         -2.31
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0221
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         12898
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0234
_refine_ls_shift/su_max          0.0048176
_refine_ls_shift/su_mean         0.0001913
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.02P)^2^ + 7.67P] 
 ,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          0.0491
_refine_ls_wR_factor_ref         0.0506
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              48
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                11262
_reflns_number_total             12928
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.17
_oxford_diffrn_Wilson_scale      323.46
_oxford_refine_ls_r_factor_ref   0.0300
_oxford_refine_ls_scale          0.057200(6)
_oxford_reflns_number_all        12898
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'CMFI_62_0m in P2(1)/c'
_cod_data_source_file            om100356a_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 21/c 1 '
_cod_original_formula_sum        'C40 H56 Cl2 N2 O2 P2 Pt1 Zr1'
_cod_database_code               4066210