Synthesis and investigation of the metal-metal interactions in early/late heterobimetallic complexes linking group 5 imido fragments to Co(i).
Evers, Deirdra A.; Bluestein, Alia H.; Foxman, Bruce M.; Thomas, Christine M.; Dalton transactions (Cambridge, England : 2003) 41 (2012) 8111–8115; doi:10.1039/c2dt00034b

data_7019195
_publ_section_title
;
 Synthesis and investigation of the metal-metal interactions in early/late
 heterobimetallic complexes linking group 5 imido fragments to Co(i).
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8111
_journal_page_last               8115
_journal_paper_doi               10.1039/c2dt00034b
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C49 H60 Co I N4 Nb P3,2(C7 H8)'
_chemical_formula_sum            'C63 H76 Co I N4 Nb P3'
_chemical_formula_weight         1260.99
_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     direct
_audit_creation_date             11-07-10
_audit_creation_method           CRYSTALS_ver_14.23
_cell_angle_alpha                90
_cell_angle_beta                 95.274(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1155(4)
_cell_length_b                   18.2831(6)
_cell_length_c                   25.2678(8)
_cell_measurement_reflns_used    9824
_cell_measurement_temperature    120
_cell_measurement_theta_max      329.96
_cell_measurement_theta_min      2.60
_cell_volume                     6033.4(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 0.996
_diffrn_measured_fraction_theta_max 0.994
_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  0.046
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            71799
_diffrn_reflns_theta_full        29.450
_diffrn_reflns_theta_max         30.051
_diffrn_reflns_theta_min         1.619
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.097
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.46
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.439
_exptl_crystal_size_mid          0.342
_exptl_crystal_size_min          0.130
_refine_diff_density_max         1.38
_refine_diff_density_min         -1.22
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         17598
_refine_ls_number_restraints     90
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.0046685
_refine_ls_shift/su_mean         0.0001712
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.03P)^2^ +13.12P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0992
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0992
_reflns_limit_h_max              18
_reflns_limit_h_min              -18
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              35
_reflns_limit_l_min              0
_reflns_number_gt                13273
_reflns_number_total             17598
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.69
_oxford_diffrn_Wilson_scale      406.42
_oxford_refine_ls_r_factor_ref   0.0568
_oxford_refine_ls_scale          0.050160(4)
_oxford_reflns_number_all        17598
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'de1_17_0m in P2(1)/c'
_cod_data_source_file            c2dt00034b.txt
_cod_data_source_block           2Nb
_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.

'_atom_sites_solution_primary' value 'Direct' changed to
'direct' 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 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C63 H76 Co1 I1 N4 Nb1 P3'
_cod_database_code               7019195
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S
RIDE C ( 2,X'S) H ( 21,X'S)
RIDE C ( 3,X'S) H ( 31,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
RIDE C ( 5,X'S) H ( 51,X'S)
RIDE C ( 6,X'S) H ( 61,X'S)
RIDE C ( 8,X'S) H ( 81,X'S)
RIDE C ( 9,X'S) H ( 91,X'S)
RIDE C ( 10,X'S) H ( 101,X'S)
RIDE C ( 11,X'S) H ( 111,X'S)
RIDE C ( 12,X'S) H ( 121,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 ( 152,X'S) H ( 151,X'S) H ( 153,X'S)
RIDE C ( 17,X'S) H ( 171,X'S)
RIDE C ( 18,X'S) H ( 181,X'S)
RIDE C ( 19,X'S) H ( 191,X'S)
RIDE C ( 20,X'S) H ( 201,X'S)
RIDE C ( 21,X'S) H ( 211,X'S)
RIDE C ( 23,X'S) H ( 231,X'S)
RIDE C ( 24,X'S) H ( 241,X'S)
RIDE C ( 25,X'S) H ( 251,X'S)
RIDE C ( 26,X'S) H ( 261,X'S)
RIDE C ( 27,X'S) H ( 271,X'S)
RIDE C ( 28,X'S) H ( 281,X'S)
RIDE C ( 29,X'S) H ( 293,X'S) H ( 292,X'S) H ( 291,X'S)
RIDE C ( 30,X'S) H ( 302,X'S) H ( 303,X'S) H ( 301,X'S)
RIDE C ( 32,X'S) H ( 321,X'S)
RIDE C ( 33,X'S) H ( 331,X'S)
RIDE C ( 34,X'S) H ( 341,X'S)
RIDE C ( 35,X'S) H ( 351,X'S)
RIDE C ( 36,X'S) H ( 361,X'S)
RIDE C ( 38,X'S) H ( 381,X'S)
RIDE C ( 39,X'S) H ( 391,X'S)
RIDE C ( 40,X'S) H ( 401,X'S)
RIDE C ( 41,X'S) H ( 411,X'S)
RIDE C ( 42,X'S) H ( 421,X'S)
RIDE C ( 43,X'S) H ( 431,X'S)
RIDE C ( 44,X'S) H ( 441,X'S) H ( 443,X'S) H ( 442,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) H ( 472,X'S) H ( 473,X'S)
RIDE C ( 48,X'S) H ( 481,X'S) H ( 483,X'S) H ( 482,X'S)
RIDE C ( 49,X'S) H ( 492,X'S) H ( 493,X'S) H ( 491,X'S)
RIDE C ( 50,X'S) H ( 501,X'S) H ( 502,X'S) H ( 503,X'S)
RIDE C ( 52,X'S) H ( 521,X'S)
RIDE C ( 53,X'S) H ( 531,X'S)
RIDE C ( 54,X'S) H ( 541,X'S)
RIDE C ( 55,X'S) H ( 551,X'S)
RIDE C ( 56,X'S) H ( 561,X'S)
RIDE C ( 57,X'S) H ( 571,X'S) H ( 572,X'S) H ( 573,X'S)
RIDE C ( 59,X'S) H ( 591,X'S)
RIDE C ( 60,X'S) H ( 601,X'S)
RIDE C ( 61,X'S) H ( 611,X'S)
RIDE C ( 62,X'S) H ( 621,X'S)
RIDE C ( 63,X'S) H ( 631,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
NO
DISTANCE 1.390000 , 0.010000 = C(51) TO C(56)
DISTANCE 1.390000 , 0.010000 = C(51) TO C(52)
DISTANCE 1.390000 , 0.010000 = C(52) TO C(53)
DISTANCE 1.390000 , 0.010000 = C(53) TO C(54)
DISTANCE 1.390000 , 0.010000 = C(54) TO C(55)
DISTANCE 1.390000 , 0.010000 = C(55) TO C(56)
U(IJ)'S 0.0, 0.010000 = C(51) TO C(56)
U(IJ)'S 0.0, 0.010000 = C(51) TO C(52)
U(IJ)'S 0.0, 0.010000 = C(52) TO C(53)
U(IJ)'S 0.0, 0.010000 = C(53) TO C(54)
U(IJ)'S 0.0, 0.010000 = C(54) TO C(55)
U(IJ)'S 0.0, 0.010000 = C(55) TO C(56)
U(IJ)'S 0.0, 0.005000 = C(50) TO C(51)
DISTANCE 1.390000 , 0.010000 = C(58) TO C(63)
DISTANCE 1.390000 , 0.010000 = C(58) TO C(59)
DISTANCE 1.390000 , 0.010000 = C(59) TO C(60)
DISTANCE 1.390000 , 0.010000 = C(60) TO C(61)
DISTANCE 1.390000 , 0.010000 = C(61) TO C(62)
DISTANCE 1.390000 , 0.010000 = C(62) TO C(63)
U(IJ)'S 0.0, 0.010000 = C(57) TO C(58)
U(IJ)'S 0.0, 0.010000 = C(58) TO C(59)
U(IJ)'S 0.0, 0.010000 = C(59) TO C(60)
U(IJ)'S 0.0, 0.010000 = C(60) TO C(61)
U(IJ)'S 0.0, 0.010000 = C(61) TO C(62)
U(IJ)'S 0.0, 0.010000 = C(62) TO C(62)
U(IJ)'S 0.0, 0.005000 = C(57) TO C(62)
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;