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_7003289
_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_sum            'C46 H68 Mo2 N4 O7'
_chemical_formula_weight         980.92
_chemical_name_systematic
;
?
;
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_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                66.083(3)
_cell_angle_beta                 74.895(3)
_cell_angle_gamma                68.780(5)
_cell_formula_units_Z            1
_cell_length_a                   9.311(1)
_cell_length_b                   11.735(1)
_cell_length_c                   12.973(1)
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_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.04
_cell_volume                     1197.09(19)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measurement_device       'Nonius Kappa CCD'
_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  0.028
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
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_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
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_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    0.574
_exptl_absorpt_correction_T_max  0.918
_exptl_absorpt_correction_T_min  0.874
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.774
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
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_refine_ls_restrained_S_obs      1.071
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.058
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0432P)^2^+0.8717P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0818
_refine_ls_wR_factor_ref         0.0797
_reflns_number_gt                5005
_reflns_number_total             5452
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b715258b.txt
_cod_data_source_block           Chisholm1144
_cod_original_cell_volume        1197.1(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7003289