Amidinate–carboxylate complexes of dimolybdenum and ditungsten: M2(O2CR)2((NiPr)2CR′)2. Preparations, molecular and electronic structures and reactions
Brown, Douglas J.; Chisholm, Malcolm H.; Gallucci, Judith C.; Dalton Transactions  (2008) 1615–1624; doi:10.1039/b715258b

data_7003287
_publ_section_title
;
 Amidinate--carboxylate complexes of dimolybdenum and ditungsten:
 M2(O2CR)2((NiPr)2CR&#x2032;)2. Preparations, molecular and electronic
 structures and reactions
;
_journal_issue                   12
_journal_name_full               'Dalton Transactions'
_journal_page_first              1615
_journal_page_last               1624
_journal_paper_doi               10.1039/b715258b
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C30 H50 Li2 N4 O2 S2'
_chemical_formula_sum            'C30 H50 Li2 N4 O2 S2'
_chemical_formula_weight         576.76
_chemical_name_common            'Chisholm 1135'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2007-01-17T16:37:54-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 95.9532(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.1730(1)
_cell_length_b                   10.9696(1)
_cell_length_c                   17.1896(2)
_cell_measurement_reflns_used    3201
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.037
_cell_measurement_wavelength     0.71073
_cell_volume                     1720.36(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.297104E-1
_diffrn_orient_matrix_UB_12      0.643002E-1
_diffrn_orient_matrix_UB_13      -0.836445E-1
_diffrn_orient_matrix_UB_21      -0.785533E-1
_diffrn_orient_matrix_UB_22      -0.456899E-1
_diffrn_orient_matrix_UB_23      -0.72212E-2
_diffrn_orient_matrix_UB_31      -0.265986E-1
_diffrn_orient_matrix_UB_32      0.405648E-1
_diffrn_orient_matrix_UB_33      0.326819E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.036
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27382
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         2.21
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.185
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.113
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'triangular plate'
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.189
_refine_diff_density_min         -0.185
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.04
_refine_ls_goodness_of_fit_gt    1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         3031
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.05
_refine_ls_restrained_S_gt       1.131
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0726P)^2^+0.4112P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1361
_refine_ls_wR_factor_gt          0.1249
_reflns_number_gt                2261
_reflns_number_total             3031
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b715258b.txt
_cod_data_source_block           Chisholm1135
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7003287