Molybdenum Oxo and Imido Complexes of β-Diketiminate Ligands: Synthesis and Structural Aspects
Ganna Lyashenko; Regine Herbst-Irmer; Vojtech Jancik; Aritra Pal; Nadia C. Mösch-Zanetti; Inorganic Chemistry 47 (2008) 113–120; doi:10.1021/ic701534a

data_4304116
_publ_section_title
;
Molybdenum Oxo and Imido Complexes of \b-Diketiminate Ligands: Synthesis
and Structural Aspects
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              113
_journal_page_last               120
_journal_paper_doi               10.1021/ic701534a
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C37 H43 Cl Mo N4, C4 H8 O'
_chemical_formula_sum            'C41 H51 Cl Mo N4 O'
_chemical_formula_weight         747.25
_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                84.18(3)
_cell_angle_beta                 79.16(3)
_cell_angle_gamma                83.00(3)
_cell_formula_units_Z            2
_cell_length_a                   8.747(2)
_cell_length_b                   10.923(2)
_cell_length_c                   19.725(4)
_cell_measurement_reflns_used    5784
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      58.99
_cell_measurement_theta_min      2.29
_cell_volume                     1831.2(7)
_computing_cell_refinement       'Bruker AXS SAINT (v 7.01A, Bruker 2003)'
_computing_data_collection       'Proteum (v 1.40, Bruker 2002)'
_computing_data_reduction        'Bruker AXS SAINT (v 7.01A, Bruker 2003)'
_computing_molecular_graphics    'Bruker AXS SHELXTL (v 6.12)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.602
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker three circle diffractometer'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  'mirror system'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0300
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            32292
_diffrn_reflns_theta_full        58.99
_diffrn_reflns_theta_max         58.99
_diffrn_reflns_theta_min         2.29
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.883
_exptl_absorpt_correction_T_max  0.6974
_exptl_absorpt_correction_T_min  0.3887
_exptl_absorpt_process_details   'Twinabs, Sheldrick 2007'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         5099
_refine_ls_number_restraints     196
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0250
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0231P)^2^+2.0234P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0646
_refine_ls_wR_factor_ref         0.0649
_reflns_number_gt                4989
_reflns_number_total             5099
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701534a-file003.cif
_cod_data_source_block           twin4o
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_database_code               4304116