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_7019197
_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_absolute_configuration ad
_chemical_formula_moiety         'C69 H100 Co1 N6 Na1 Nb1 O5 P3'
_chemical_formula_sum            'C69 H100 Co N6 Na Nb O5 P3'
_chemical_formula_weight         1361.34
_space_group_IT_number           1
_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             11-07-14
_audit_creation_method           CRYSTALS_ver_14.23
_cell_angle_alpha                91.900(2)
_cell_angle_beta                 117.275(2)
_cell_angle_gamma                112.938(2)
_cell_formula_units_Z            1
_cell_length_a                   12.8515(4)
_cell_length_b                   12.9728(5)
_cell_length_c                   13.2306(4)
_cell_measurement_reflns_used    8993
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     1744.07(12)
_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    'USER DEFINED STRUCTURE SOLUTION'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.043
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            35556
_diffrn_reflns_theta_full        30.074
_diffrn_reflns_theta_max         30.074
_diffrn_reflns_theta_min         1.884
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.529
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Analytical Absorption (De Meulenaer & Tompa, 1965)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'plate fragment'
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.396
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.095
_refine_diff_density_max         0.73
_refine_diff_density_min         -0.64
_refine_ls_abs_structure_details 'Flack (1983), 3625 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.015(11)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9935
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     764
_refine_ls_number_reflns         13788
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.0155579
_refine_ls_shift/su_mean         0.0006315
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 0.31P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0884
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0884
_reflns_limit_h_max              17
_reflns_limit_h_min              -18
_reflns_limit_k_max              18
_reflns_limit_k_min              -17
_reflns_limit_l_max              18
_reflns_limit_l_min              -18
_reflns_number_gt                12445
_reflns_number_total             13788
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.64
_oxford_diffrn_Wilson_scale      1.22
_oxford_refine_ls_r_factor_ref   0.0416
_oxford_refine_ls_scale          0.21781(7)
_oxford_reflns_number_all        13788
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'DE1_24_0m in P1'
_cod_data_source_file            c2dt00034b.txt
_cod_data_source_block           3Nb
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 'Other' changed to
'other' 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 '
_cod_original_formula_sum        'C69 H100 Co1 N6 Na1 Nb1 O5 P3'
_cod_database_code               7019197
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE NB(1,X'S, U'S ) UNTIL C(69)
CONT C(500,X'S,U[ISO]) UNTIL C(681)
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 ( 151,X'S) H ( 152,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 ( 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 ( 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 ( 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) H ( 472,X'S) H ( 473,X'S)
RIDE C ( 48,X'S) H ( 481,X'S) H ( 482,X'S) H ( 483,X'S)
RIDE C ( 49,X'S) H ( 491,X'S) H ( 492,X'S) H ( 493,X'S)
RIDE C ( 500,X'S) H ( 5001,X'S) H ( 5002,X'S)
RIDE C ( 501,X'S) H ( 5011,X'S) H ( 5012,X'S)
REM TOO MANY H ATOMS ON C ( 57), - 4
RIDE C ( 57,X'S) H ( 571,X'S) H ( 572,X'S)
CONT H ( 573,X'S) H ( 574,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)
RIDE C ( 60,X'S) H ( 601,X'S) H ( 602,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)
RIDE C ( 65,X'S) H ( 651,X'S) H ( 652,X'S)
REM TOO MANY H ATOMS ON C ( 69), - 4
RIDE C ( 69,X'S) H ( 691,X'S) H ( 692,X'S)
CONT H ( 693,X'S) H ( 694,X'S)
RIDE C ( 510,X'S) H (5101,X'S) H (5102,X'S)
RIDE C ( 511,X'S) H (5111,X'S) H (5112,X'S)
RIDE C ( 520,X'S) H (5201,X'S) H (5202,X'S)
RIDE C ( 521,X'S) H (5211,X'S) H (5212,X'S)
RIDE C ( 530,X'S) H (5301,X'S) H (5302,X'S)
RIDE C ( 531,X'S) H (5311,X'S) H (5312,X'S)
RIDE C ( 540,X'S) H (5401,X'S) H (5402,X'S)
RIDE C ( 541,X'S) H (5411,X'S) H (5412,X'S)
RIDE C ( 550,X'S) H (5501,X'S) H (5502,X'S)
RIDE C ( 551,X'S) H (5511,X'S) H (5512,X'S)
RIDE C ( 560,X'S) H (5601,X'S) H (5602,X'S)
RIDE C ( 561,X'S) H (5611,X'S) H (5612,X'S)
RIDE C ( 640,X'S) H (6401,X'S) H (6402,X'S)
RIDE C ( 641,X'S) H (6411,X'S) H (6412,X'S)
RIDE C ( 660,X'S) H (6601,X'S) H (6602,X'S)
RIDE C ( 661,X'S) H (6611,X'S) H (6612,X'S)
RIDE C ( 670,X'S) H (6701,X'S) H (6702,X'S)
RIDE C ( 671,X'S) H (6711,X'S) H (6712,X'S)
RIDE C ( 680,X'S) H (6801,X'S) H (6802,X'S)
RIDE C ( 681,X'S) H (6811,X'S) H (6812,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
;