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_4328920
_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         'C27 H32 Mo N2 O4, C4 H8 O'
_chemical_formula_sum            'C31 H40 Mo N2 O5'
_chemical_formula_weight         616.59
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.979(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.1441(6)
_cell_length_b                   23.6151(16)
_cell_length_c                   15.1751(10)
_cell_measurement_reflns_used    14014
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.15
_cell_measurement_theta_min      2.5
_cell_volume                     2914.6(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, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'STOE IPDS 2T'
_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  0.0987
_diffrn_reflns_av_sigmaI/netI    0.1081
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14882
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.78
_diffrn_reflns_theta_min         4.72
_exptl_absorpt_coefficient_mu    0.492
_exptl_absorpt_correction_T_max  1.1091
_exptl_absorpt_correction_T_min  0.8553
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       needle
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.792
_refine_diff_density_min         -1.473
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         6041
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.1028
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0742P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1238
_refine_ls_wR_factor_ref         0.1438
_reflns_number_gt                3879
_reflns_number_total             6041
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic202517w_si_001_05.cif
_cod_data_source_block           compound4
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4328920