Molybdenum 1,4-Diazabuta-1,3-diene Tricarbonyl Solvento Complexes Revisited: From Solvatochromism to Attractive Ligand-Ligand Interaction
Benjamin Oelkers; Alexander Venker; Jörg Sundermeyer; Inorganic Chemistry 51 (2012) 4636–4643; doi:10.1021/ic202517w

data_4328933
_publ_section_title
;
 Molybdenum 1,4-Diazabuta-1,3-diene Tricarbonyl Solvento Complexes
 Revisited: From Solvatochromism to Attractive Ligand-Ligand Interaction
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4636
_journal_page_last               4643
_journal_paper_doi               10.1021/ic202517w
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C47 H48 Mo2 N5 O6, C8 H20 N, C H2 Cl2'
_chemical_formula_sum            'C56 H70 Cl2 Mo2 N6 O6'
_chemical_formula_weight         1185.96
_chemical_name_systematic
;
 ?
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.615(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.8000(6)
_cell_length_b                   14.5851(3)
_cell_length_c                   21.3420(6)
_cell_measurement_reflns_used    32495
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.2
_cell_measurement_theta_min      1.69
_cell_volume                     5800.4(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2011)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Giacovazzo et al, 2004)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_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  0.1289
_diffrn_reflns_av_sigmaI/netI    0.0931
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            73410
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.75
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.576
_exptl_absorpt_correction_T_max  0.9543
_exptl_absorpt_correction_T_min  0.8978
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
a grid of  8 x  8 x  8 =   512 sampling points was used
;
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_description       block
_exptl_crystal_F_000             2456
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.742
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.803
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     751
_refine_ls_number_reflns         12302
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      0.801
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0792
_refine_ls_wR_factor_ref         0.0836
_reflns_number_gt                7833
_reflns_number_total             12302
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic202517w_si_001_18.cif
_cod_data_source_block           compound19
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4328933