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_7028874
_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         'C46 H77 Co1 N5 O1 P3 Zr1'
_chemical_formula_sum            'C46 H77 Co N5 O P3 Zr'
_chemical_formula_weight         959.22
_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   difmap
_atom_sites_solution_primary     other
_audit_creation_date             12-07-16
_audit_creation_method           CRYSTALS_ver_14.41
_cell_angle_alpha                90
_cell_angle_beta                 106.602(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.9948(17)
_cell_length_b                   22.4923(17)
_cell_length_c                   19.5321(14)
_cell_measurement_reflns_used    9917
_cell_measurement_temperature    120
_cell_measurement_theta_max      29
_cell_measurement_theta_min      3
_cell_volume                     9681.0(13)
_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 0.999
_diffrn_measured_fraction_theta_max 0.992
_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  0.071
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            110797
_diffrn_reflns_theta_full        28.509
_diffrn_reflns_theta_max         29.091
_diffrn_reflns_theta_min         1.848
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.696
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4064
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.160
_refine_diff_density_max         1.63
_refine_diff_density_min         -1.16
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1025
_refine_ls_number_reflns         25761
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.0141503
_refine_ls_shift/su_mean         0.0024257
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 9.30P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1006
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.1006
_reflns_limit_h_max              30
_reflns_limit_h_min              -31
_reflns_limit_k_max              30
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                15829
_reflns_number_total             25761
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0835
_oxford_refine_ls_scale          0.0360787(17)
_oxford_reflns_number_all        25761
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'ZW_570_0ma in P2(1)/c'
_cod_data_source_file            c3dt52133h.txt
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/usr/data/users/saulius/automatic-downloads/current/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 
;
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C46 H77 Co1 N5 O1 P3 Zr1'
_cod_database_code               7028874
_iucr_refine_instructions_details_constraints
;
BLOCK 
CONT SCALE 
CONT ZR   (    1 ,X'S,U'S)  UNTIL C    (   40 ) 
CONT C    (   41 ,X'S,U[ISO])  UNTIL C    (   44 ) 
CONT C    (   45 ,X'S,U'S)  UNTIL C    (  136 ) 
CONT C    (  137 ,X'S,U[ISO])  UNTIL C    (  138 ) 
CONT C    (  139 ,X'S,U'S) 
CONT C    (  140 ,X'S,U[ISO])  UNTIL C    (  141 ) 
CONT C    (  142 ,X'S,U'S)  UNTIL C    (  148 ) 
SUMFIX PART(1001, OCC) AND PART(1002, OCC) 
SUMFIX PART(1003, OCC) AND PART(1004, OCC) 
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   (  71,X'S) H   (  72,X'S) H   (  73,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   ( 101,X'S) H   ( 102,X'S) H   ( 103,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) H   ( 112,X'S) H   ( 113,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) H   ( 132,X'S) H   ( 133,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 142,X'S) H   ( 143,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   ( 211,X'S) H   ( 212,X'S) H   ( 213,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S) H   ( 223,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   ( 251,X'S) H   ( 252,X'S) H   ( 253,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) H   ( 272,X'S) H   ( 273,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) H   ( 282,X'S) H   ( 283,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   ( 351,X'S) H   ( 352,X'S) H   ( 353,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 362,X'S) H   ( 363,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) H   ( 382,X'S) H   ( 383,X'S) 
RIDE C   (  39,X'S) H   ( 392,X'S) H   ( 393,X'S) H   ( 396,X'S) 
RIDE C   (  40,X'S) H   ( 443,X'S) H   ( 445,X'S) H   ( 446,X'S) 
CONT H   ( 441,X'S) H   ( 442,X'S) H   ( 444,X'S) 
RIDE C   (  41,X'S) H   ( 421,X'S) 
RIDE C   (  42,X'S) H   ( 431,X'S) H   ( 432,X'S) H   ( 433,X'S) 
RIDE C   (  43,X'S) H   ( 451,X'S) 
RIDE C   (  44,X'S) H   ( 461,X'S) H   ( 462,X'S) H   ( 463,X'S) 
RIDE C   (  45,X'S) H   ( 501,X'S) H   ( 502,X'S) 
RIDE C   (  46,X'S) H   ( 491,X'S) H   ( 492,X'S) 
RIDE C   (  47,X'S) H   ( 481,X'S) H   ( 482,X'S) 
RIDE C   (  48,X'S) H   ( 471,X'S) H   ( 472,X'S) 
RIDE C   ( 102,X'S) H   (1021,X'S) 
RIDE C   ( 104,X'S) H   (1041,X'S) 
RIDE C   ( 106,X'S) H   (1061,X'S) 
RIDE C   ( 107,X'S) H   (1071,X'S) H   (1072,X'S) H   (1073,X'S) 
RIDE C   ( 108,X'S) H   (1081,X'S) H   (1082,X'S) H   (1083,X'S) 
RIDE C   ( 109,X'S) H   (1091,X'S) 
RIDE C   ( 110,X'S) H   (1101,X'S) H   (1102,X'S) H   (1103,X'S) 
RIDE C   ( 111,X'S) H   (1111,X'S) H   (1112,X'S) H   (1113,X'S) 
RIDE C   ( 112,X'S) H   (1121,X'S) 
RIDE C   ( 113,X'S) H   (1131,X'S) H   (1132,X'S) H   (1133,X'S) 
RIDE C   ( 114,X'S) H   (1141,X'S) H   (1142,X'S) H   (1143,X'S) 
RIDE C   ( 116,X'S) H   (1161,X'S) 
RIDE C   ( 118,X'S) H   (1181,X'S) 
RIDE C   ( 120,X'S) H   (1201,X'S) 
RIDE C   ( 121,X'S) H   (1211,X'S) H   (1212,X'S) H   (1213,X'S) 
RIDE C   ( 122,X'S) H   (1221,X'S) H   (1222,X'S) H   (1223,X'S) 
RIDE C   ( 123,X'S) H   (1231,X'S) 
RIDE C   ( 124,X'S) H   (1241,X'S) H   (1242,X'S) H   (1243,X'S) 
RIDE C   ( 125,X'S) H   (1251,X'S) H   (1252,X'S) H   (1253,X'S) 
RIDE C   ( 126,X'S) H   (1261,X'S) 
RIDE C   ( 127,X'S) H   (1271,X'S) H   (1272,X'S) H   (1273,X'S) 
RIDE C   ( 128,X'S) H   (1281,X'S) H   (1282,X'S) H   (1283,X'S) 
RIDE C   ( 130,X'S) H   (1301,X'S) 
RIDE C   ( 132,X'S) H   (1321,X'S) 
RIDE C   ( 134,X'S) H   (1341,X'S) 
RIDE C   ( 135,X'S) H   (1351,X'S) H   (1352,X'S) H   (1353,X'S) 
RIDE C   ( 136,X'S) H   (1361,X'S) H   (1362,X'S) H   (1363,X'S) 
RIDE C   ( 137,X'S) H   (1371,X'S) 
RIDE C   ( 138,X'S) H   (1381,X'S) H   (1382,X'S) H   (1383,X'S) 
RIDE C   ( 139,X'S) H   (1391,X'S) H   (1392,X'S) H   (1394,X'S) 
CONT H   (1393,X'S) H   (1395,X'S) H   (1396,X'S) 
RIDE C   ( 140,X'S) H   (1401,X'S) 
RIDE C   ( 141,X'S) H   (1411,X'S) H   (1412,X'S) H   (1413,X'S) 
RIDE C   ( 142,X'S) H   (1421,X'S) 
RIDE C   ( 143,X'S) H   (1431,X'S) H   (1432,X'S) H   (1433,X'S) 
RIDE C   ( 144,X'S) H   (1441,X'S) H   (1442,X'S) H   (1443,X'S) 
RIDE C   ( 145,X'S) H   (1451,X'S) H   (1452,X'S) 
RIDE C   ( 146,X'S) H   (1461,X'S) H   (1462,X'S) 
RIDE C   ( 147,X'S) H   (1471,X'S) H   (1472,X'S) 
RIDE C   ( 148,X'S) H   (1481,X'S) H   (1482,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                                                                             
;