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_7003291
_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_formula_moiety         'C42 H52 Fe2 Mo2 N4 O4, 4(C4 H8 O)'
_chemical_formula_sum            'C58 H84 Fe2 Mo2 N4 O8'
_chemical_formula_weight         1268.87
_chemical_name_systematic
;
?
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                67.157(1)
_cell_angle_beta                 78.161(1)
_cell_angle_gamma                85.503(1)
_cell_formula_units_Z            1
_cell_length_a                   11.1354(1)
_cell_length_b                   11.8625(1)
_cell_length_c                   12.3209(1)
_cell_measurement_reflns_used    6696
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.04
_cell_volume                     1467.96(2)
_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_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            40640
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    0.956
_exptl_absorpt_correction_T_max  0.892
_exptl_absorpt_correction_T_min  0.804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rhombus-shaped plate'
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.232
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         6736
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0768P)^2^+0.9273P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1248
_reflns_number_gt                5529
_reflns_number_total             6736
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b715258b.txt
_cod_data_source_block           Chisholm1272
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7003291