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_7109192
_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         'C49 H88 Co1 N7 O1 P3 Zr1'
_chemical_formula_sum            'C49 H88 Co N7 O P3 Zr'
_chemical_formula_weight         1034.36
_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     direct
_audit_creation_date             11-07-14
_audit_creation_method           CRYSTALS_ver_14.23
_cell_angle_alpha                97.3550(10)
_cell_angle_beta                 96.2060(10)
_cell_angle_gamma                94.278(2)
_cell_formula_units_Z            2
_cell_length_a                   12.1683(4)
_cell_length_b                   12.8589(4)
_cell_length_c                   17.2789(5)
_cell_measurement_reflns_used    9794
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     2654.94(14)
_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 0.997
_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  0.039
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            78463
_diffrn_reflns_theta_full        29.454
_diffrn_reflns_theta_max         30.055
_diffrn_reflns_theta_min         1.864
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.640
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Analytical Absorption (De Meulenaer & Tompa, 1965)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1102
_exptl_crystal_size_max          0.319
_exptl_crystal_size_mid          0.238
_exptl_crystal_size_min          0.128
_refine_diff_density_max         0.79
_refine_diff_density_min         -0.46
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9711
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         15426
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0265
_refine_ls_shift/su_max          0.0024413
_refine_ls_shift/su_mean         0.0000507
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 1.49P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0655
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0655
_reflns_limit_h_max              16
_reflns_limit_h_min              -17
_reflns_limit_k_max              17
_reflns_limit_k_min              -18
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                12688
_reflns_number_total             15426
_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   0.0352
_oxford_refine_ls_scale          0.14663(2)
_oxford_reflns_number_all        15426
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'jwn_114_0m in P-1'
_cod_data_source_file            c2cc35594a.txt
_cod_data_source_block           jwn_114
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Direct' changed to 'direct'
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_H-M      'P -1 '
_cod_original_formula_sum        'C49 H88 Co1 N7 O1 P3 Zr1'
_cod_database_code               7109192
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S
RIDE N ( 6,X'S) H ( 64,X'S)
RIDE N ( 7,X'S) H ( 71,X'S) H ( 72,X'S)
RIDE C ( 1,X'S) H ( 11,X'S)
RIDE C ( 2,X'S) H ( 21,X'S) H ( 22,X'S) H ( 23,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 ( 41,X'S)
RIDE C ( 5,X'S) H ( 51,X'S) H ( 52,X'S) H ( 53,X'S)
RIDE C ( 6,X'S) H ( 61,X'S) H ( 62,X'S) H ( 63,X'S)
RIDE C ( 9,X'S) H ( 91,X'S)
RIDE C ( 11,X'S) H ( 111,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 ( 15,X'S) H ( 151,X'S) H ( 152,X'S) H ( 153,X'S)
RIDE C ( 16,X'S) H ( 161,X'S)
RIDE C ( 17,X'S) H ( 171,X'S) H ( 172,X'S) H ( 173,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 ( 20,X'S) H ( 201,X'S) H ( 202,X'S) H ( 203,X'S)
RIDE C ( 21,X'S) H ( 211,X'S) H ( 212,X'S) H ( 213,X'S)
RIDE C ( 24,X'S) H ( 241,X'S)
RIDE C ( 26,X'S) H ( 261,X'S)
RIDE C ( 28,X'S) H ( 281,X'S) H ( 282,X'S) H ( 283,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 ( 31,X'S) H ( 311,X'S)
RIDE C ( 32,X'S) H ( 321,X'S) H ( 322,X'S) H ( 323,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 ( 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 ( 39,X'S) H ( 391,X'S)
RIDE C ( 41,X'S) H ( 411,X'S)
RIDE C ( 43,X'S) H ( 431,X'S) H ( 432,X'S) H ( 433,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 ( 46,X'S) H ( 461,X'S) H ( 462,X'S) H ( 463,X'S)
RIDE C ( 47,X'S) H ( 471,X'S) H ( 472,X'S)
RIDE C ( 48,X'S) H ( 481,X'S) H ( 482,X'S)
RIDE C ( 49,X'S) H ( 491,X'S) H ( 492,X'S) H ( 493,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;