Effect of ligand modification on the reactivity of phosphinoamide-bridged heterobimetallic Zr/Co complexes.
Zhou, Wen; Saper, Noam I.; Krogman, Jeremy P.; Foxman, Bruce M.; Thomas, Christine M.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 1984–1989; doi:10.1039/c3dt52133h

data_7028875
_publ_section_title
;
 Effect of ligand modification on the reactivity of phosphinoamide-bridged
 heterobimetallic Zr/Co complexes.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1984
_journal_page_last               1989
_journal_paper_doi               10.1039/c3dt52133h
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C42 H69 Br2 Co1 N3 P3 Zr1'
_chemical_formula_sum            'C42 H69 Br2 Co N3 P3 Zr'
_chemical_formula_weight         1018.91
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             13-04-15
_audit_creation_method           CRYSTALS_ver_14.41
_cell_angle_alpha                90
_cell_angle_beta                 97.6840(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0391(3)
_cell_length_b                   19.7151(5)
_cell_length_c                   21.9331(6)
_cell_measurement_reflns_used    9875
_cell_measurement_temperature    135
_cell_measurement_theta_max      28
_cell_measurement_theta_min      3
_cell_volume                     5159.1(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      135
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.042
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12445
_diffrn_reflns_theta_full        28.004
_diffrn_reflns_theta_max         28.004
_diffrn_reflns_theta_min         1.394
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.194
_exptl_absorpt_correction_T_max  0.67
_exptl_absorpt_correction_T_min  0.55
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'prism fragment'
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.279
_exptl_crystal_size_mid          0.276
_exptl_crystal_size_min          0.184
_platon_squeeze_details
;
During the structure solution, electron density difference maps
revealed that there were disordered solvent molecule(s) which
could not be successfully modeled.  The pentane solvate was 
highly disordered in a volume PLATON SQUEEZE reported to be
704.8 \%A3 per unit cell (13.6%). It appeared that the cavity area
contained ca. tfour pentane molecules, located near a center of 
symmetry at (0, 0, 0) and (0, 1/2, 1/2). 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.
PLATON reported a total electron density of 158 e- per unit cell, 
likely representing four 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         1.30
_refine_diff_density_min         -1.07
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9491
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         12445
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0291
_refine_ls_shift/su_max          0.0019913
_refine_ls_shift/su_mean         0.0000439
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 4.30P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0713
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0713
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                9631
_reflns_number_total             12445
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.74
_oxford_diffrn_Wilson_scale      221.77
_oxford_refine_ls_r_factor_ref   0.0440
_oxford_refine_ls_scale          0.072012(7)
_oxford_reflns_number_all        12445
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'ZW_595_0m in P2(1)/n'
_cod_data_source_file            c3dt52133h.txt
_cod_data_source_block           5
_cod_original_sg_symbol_Hall     -P2yn
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C42 H69 Br2 Co1 N3 P3 Zr1'
_cod_database_code               7028875
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   7,X'S) H   (  73,X'S) H   (  72,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) H   (  82,X'S) H   (  83,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 102,X'S) H   ( 101,X'S) H   ( 103,X'S) 
RIDE C   (  11,X'S) H   ( 112,X'S) H   ( 113,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 132,X'S) H   ( 131,X'S) H   ( 133,X'S) 
RIDE C   (  14,X'S) H   ( 142,X'S) H   ( 143,X'S) H   ( 141,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 213,X'S) H   ( 211,X'S) H   ( 212,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 223,X'S) H   ( 222,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) H   ( 243,X'S) 
RIDE C   (  25,X'S) H   ( 252,X'S) H   ( 253,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 273,X'S) H   ( 271,X'S) H   ( 272,X'S) 
RIDE C   (  28,X'S) H   ( 282,X'S) H   ( 283,X'S) H   ( 281,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 352,X'S) H   ( 351,X'S) H   ( 353,X'S) 
RIDE C   (  36,X'S) H   ( 363,X'S) H   ( 361,X'S) H   ( 362,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  38,X'S) H   ( 383,X'S) H   ( 381,X'S) H   ( 382,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) H   ( 393,X'S) H   ( 392,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) H   ( 413,X'S) H   ( 412,X'S) 
RIDE C   (  42,X'S) H   ( 422,X'S) H   ( 421,X'S) H   ( 423,X'S) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;