N-H activation of hydrazines by a heterobimetallic Zr-Co complex: promotion of one-electron chemistry at Zr
J. W. Napoline; Mark W. Bezpalko; Bruce M. Foxmana; Christine M. Thomas; Chem.Commun. 49 (2013) 4388–; doi:10.1039/c2cc35594a

data_7109191
_publ_section_title
;
 N-H activation of hydrazines by a heterobimetallic Zr-Co complex:
 promotion of one-electron chemistry at Zr
;
_journal_name_full               Chem.Commun.
_journal_page_first              4388
_journal_paper_doi               10.1039/c2cc35594a
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C57 H97 Co1 N7 O1.50 P3 Zr1'
_chemical_formula_sum            'C57 H97 Co N7 O1.5 P3 Zr'
_chemical_formula_weight         1147.53
_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   difmap
_atom_sites_solution_primary     other
_audit_creation_date             11-08-04
_audit_creation_method           CRYSTALS_ver_14.23
_cell_angle_alpha                97.813(3)
_cell_angle_beta                 91.737(3)
_cell_angle_gamma                104.989(3)
_cell_formula_units_Z            4
_cell_length_a                   13.6949(8)
_cell_length_b                   20.9745(12)
_cell_length_c                   21.5785(12)
_cell_measurement_reflns_used    9806
_cell_measurement_temperature    120
_cell_measurement_theta_max      29
_cell_measurement_theta_min      3
_cell_volume                     5917.9(6)
_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 0.995
_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  0.047
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            124570
_diffrn_reflns_theta_full        28.594
_diffrn_reflns_theta_max         29.177
_diffrn_reflns_theta_min         1.495
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.582
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'prism fragment'
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.433
_exptl_crystal_size_mid          0.358
_exptl_crystal_size_min          0.210
_refine_diff_density_max         1.98
_refine_diff_density_min         -1.66
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9740
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1270
_refine_ls_number_reflns         31756
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.0254272
_refine_ls_shift/su_mean         0.0002516
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.05P)^2^ +12.31P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1240
_refine_ls_wR_factor_gt          0.1134
_refine_ls_wR_factor_ref         0.1240
_reflns_limit_h_max              18
_reflns_limit_h_min              -18
_reflns_limit_k_max              28
_reflns_limit_k_min              -28
_reflns_limit_l_max              29
_reflns_limit_l_min              0
_reflns_number_gt                23306
_reflns_number_total             31756
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.69
_oxford_diffrn_Wilson_scale      77.58
_oxford_refine_ls_r_factor_ref   0.0711
_oxford_refine_ls_scale          0.078375(9)
_oxford_reflns_number_all        31756
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'jwn_148_0m in P-1'
_cod_data_source_file            c2cc35594a.txt
_cod_data_source_block           jwn_148
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C57 H97 Co1 N7 O1.50 P3 Zr1'
_cod_database_code               7109191
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S
RIDE N ( 4,X'S) H ( 41,X'S) H ( 42,X'S)
RIDE N ( 104,X'S) H (1041,X'S) H (1042,X'S)
RIDE C ( 3,X'S) H ( 31,X'S) H ( 32,X'S) H ( 33,X'S)
RIDE C ( 4,X'S) H (1512,X'S)
RIDE C ( 6,X'S) H ( 61,X'S) H ( 62,X'S) H ( 63,X'S)
RIDE C ( 7,X'S) H ( 71,X'S)
RIDE C ( 9,X'S) H ( 91,X'S) H ( 92,X'S) H ( 93,X'S)
RIDE C ( 10,X'S) H ( 101,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) H ( 122,X'S) H ( 123,X'S)
RIDE C ( 13,X'S) H ( 131,X'S)
RIDE C ( 14,X'S) H ( 141,X'S) H ( 142,X'S) H ( 143,X'S)
RIDE C ( 15,X'S) H ( 151,X'S) H ( 152,X'S) H ( 153,X'S)
RIDE C ( 18,X'S) H ( 181,X'S) H ( 182,X'S) H ( 183,X'S)
RIDE C ( 19,X'S) H ( 191,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)
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)
RIDE C ( 26,X'S) H ( 261,X'S) H ( 262,X'S) H ( 263,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)
RIDE C ( 29,X'S) H ( 291,X'S) H ( 292,X'S) H ( 293,X'S)
RIDE C ( 30,X'S) H ( 301,X'S) H ( 302,X'S) H ( 303,X'S)
RIDE C ( 33,X'S) H ( 331,X'S) H ( 332,X'S) H ( 333,X'S)
RIDE C ( 34,X'S) H ( 341,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 ( 39,X'S) H ( 391,X'S) H ( 392,X'S) H ( 393,X'S)
RIDE C ( 40,X'S) H ( 401,X'S)
RIDE C ( 41,X'S) H ( 411,X'S) H ( 412,X'S) H ( 413,X'S)
RIDE C ( 42,X'S) H ( 421,X'S) H ( 422,X'S) H ( 423,X'S)
RIDE C ( 43,X'S) H ( 431,X'S)
RIDE C ( 44,X'S) H ( 441,X'S) H ( 442,X'S) H ( 443,X'S)
RIDE C ( 45,X'S) H ( 451,X'S) H ( 452,X'S) H ( 453,X'S)
RIDE C ( 47,X'S) H ( 471,X'S)
RIDE C ( 48,X'S) H ( 481,X'S)
RIDE C ( 49,X'S) H ( 491,X'S)
RIDE C ( 50,X'S) H ( 501,X'S)
RIDE C ( 51,X'S) H ( 511,X'S)
RIDE C ( 52,X'S) H ( 521,X'S) H ( 522,X'S) H ( 523,X'S)
RIDE C ( 53,X'S) H ( 531,X'S) H ( 532,X'S)
RIDE C ( 54,X'S) H ( 541,X'S) H ( 542,X'S)
RIDE C ( 55,X'S) H ( 551,X'S) H ( 552,X'S) H ( 553,X'S)
RIDE C ( 56,X'S) H ( 561,X'S) H ( 562,X'S) H ( 563,X'S)
RIDE C ( 57,X'S) H ( 571,X'S) H ( 572,X'S)
RIDE C ( 58,X'S) H ( 581,X'S) H ( 582,X'S)
RIDE C ( 59,X'S) H ( 591,X'S) H ( 592,X'S) H ( 593,X'S)
RIDE C ( 60,X'S) H ( 601,X'S) H ( 602,X'S) H ( 603,X'S)
RIDE C ( 61,X'S) H ( 611,X'S) H ( 612,X'S)
RIDE C ( 62,X'S) H ( 621,X'S) H ( 622,X'S)
RIDE C ( 63,X'S) H ( 631,X'S) H ( 632,X'S) H ( 633,X'S)
RIDE C ( 103,X'S) H (1031,X'S) H (1032,X'S) H (1033,X'S)
RIDE C ( 104,X'S) H (1513,X'S)
RIDE C ( 106,X'S) H (1061,X'S) H (1062,X'S) H (1063,X'S)
RIDE C ( 107,X'S) H (1071,X'S)
RIDE C ( 109,X'S) H (1091,X'S) H (1092,X'S) H (1093,X'S)
RIDE C ( 110,X'S) H (1101,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) H (1122,X'S) H (1123,X'S)
RIDE C ( 113,X'S) H (1131,X'S)
RIDE C ( 114,X'S) H (1141,X'S) H (1142,X'S) H (1143,X'S)
RIDE C ( 115,X'S) H (1151,X'S) H (1152,X'S) H (1153,X'S)
RIDE C ( 118,X'S) H (1181,X'S) H (1182,X'S) H (1183,X'S)
RIDE C ( 119,X'S) H (1191,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)
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)
RIDE C ( 126,X'S) H (1261,X'S) H (1262,X'S) H (1263,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)
RIDE C ( 129,X'S) H (1291,X'S) H (1292,X'S) H (1293,X'S)
RIDE C ( 130,X'S) H (1301,X'S) H (1302,X'S) H (1303,X'S)
RIDE C ( 133,X'S) H (1331,X'S) H (1332,X'S) H (1333,X'S)
RIDE C ( 134,X'S) H (1341,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 ( 139,X'S) H (1391,X'S) H (1392,X'S) H (1393,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) H (1422,X'S) H (1423,X'S)
RIDE C ( 143,X'S) H (1431,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) H (1453,X'S)
RIDE C ( 147,X'S) H (1471,X'S)
RIDE C ( 148,X'S) H (1481,X'S)
RIDE C ( 149,X'S) H (1491,X'S)
RIDE C ( 150,X'S) H (1501,X'S)
RIDE C ( 151,X'S) H (1511,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
NO
END
;