The first molybdenum dioxo compounds with η^2^-pyrazolate ligands: crystal structure and oxo transfer properties
Most, Kerstin; Köpke, Sinje; Dall'Antonia, Fabio; Mösch-Zanetti, Nadia C.; Chemical Communications  (2002) 1676–1677; doi:10.1039/b205420e

data_7111238
_publ_section_title
;
 The first molybdenum dioxo compounds with \h^2^-pyrazolate ligands: crystal
 structure and oxo transfer properties
;
_journal_issue                   16
_journal_name_full               'Chemical Communications'
_journal_page_first              1676
_journal_page_last               1677
_journal_paper_doi               10.1039/b205420e
_journal_year                    2002
_chemical_formula_sum            'C11 H19 Cl Mo N2 O2'
_chemical_formula_weight         342.67
_chemical_name_systematic        ?
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 106.87(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.35(1)
_cell_length_b                   10.28(1)
_cell_length_c                   19.75(2)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.85
_cell_measurement_theta_min      2.98
_cell_volume                     2982(5)
_computing_cell_refinement       'Bruker AXS SAINT (V.5.00, Madison 1997)'
_computing_data_collection       'Siemens SMART (V.4.202, Siemens 1996)'
_computing_data_reduction        'Bruker AXS SAINT (V.5.00, Madison 1997)'
_computing_molecular_graphics    'Bruker AXS SHELXTL (V. 5.10)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean '8.192 pixels/mm'
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type
'STOE-Siemens-Huber four circle diffractometer'
_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  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21708
_diffrn_reflns_theta_full        27.91
_diffrn_reflns_theta_max         27.91
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.052
_exptl_absorpt_correction_T_max  0.7431
_exptl_absorpt_correction_T_min  0.5708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'Blessing, R. H. (1995). Acta Cryst. A51, 33-38'
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.11(3)
_refine_ls_extinction_coef       0.00219(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         5532
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0220
_refine_ls_R_factor_gt           0.0217
_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^)+(0.0258P)^2^+2.8463P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0545
_refine_ls_wR_factor_ref         0.0546
_reflns_number_gt                5491
_reflns_number_total             5532
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b205420esup1.cif
_cod_data_source_block           publ
_cod_original_cell_volume        2980(6)
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               7111238