Chlorobis[1,1'-diphenylhydrazido(2‒)-<i>N</i>^2^][hydridotris(pyrazolyl-<i>N</i>^2^)borato]molybdenum(VI)
Carolina Manzur; David Carrillo; Daphne Boys; Acta Crystallographica Section C 53 (1997) 1401–1403; doi:10.1107/S0108270197007452

data_2006577
_publ_section_title
Chlorobis[1,1'-diphenylhydrazido(2--)-<i>N</i>^2^][hydridotris(pyrazolyl-<i>N</i>^2^)borato]molybdenum(VI)
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1401
_journal_page_last               1403
_journal_paper_doi               10.1107/S0108270197007452
_journal_volume                  53
_journal_year                    1997
_chemical_formula_iupac          '[Mo Cl (C9 H10 B N6) (C12 H10 N1)2]'
_chemical_formula_moiety         'C33 H30 B Cl Mo N10'
_chemical_formula_structural     HB(C3H3N2)3Mo(NNC6H5)2Cl
_chemical_formula_sum            'C33 H30 B Cl Mo N10'
_chemical_formula_weight         708.87
_chemical_melting_point          520.15
_chemical_name_systematic
;
 [hydridotris(pyrazolyl)borato]-bis[1,1-diphenylhydrazido(2-)]chloromo-
 lybdenum(VI)
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 112.76(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.504(3)
_cell_length_b                   18.536(5)
_cell_length_c                   10.305(3)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      7.5
_cell_volume                     1674.0(9)
_computing_cell_refinement       P3/P4-PC
_computing_data_collection       'P3/P4-PC (Siemens, 1991)'
_computing_data_reduction        'XDISK in SHELXTL/PC (Sheldrich, 1991)'
_computing_molecular_graphics    'XP in SHELXTL/PC'
_computing_publication_material  'CIFTAB in SHELXL93'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'XS in SHELXTL/PC'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens R3m/V four-circle diffractometer'
_diffrn_measurement_method       '\q/2\q 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  0.030
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5327
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         2.14
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 98
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.511
_exptl_absorpt_correction_T_max  0.766
_exptl_absorpt_correction_T_min  0.681
_exptl_absorpt_correction_type
'\y scans (XEMP in SHELXTL/PC; Sheldrick, 1991)'
_exptl_crystal_colour            'deep orange'
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.418
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.008
_refine_ls_goodness_of_fit_obs   1.050
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         5056
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.008
_refine_ls_restrained_S_obs      1.050
_refine_ls_R_factor_all          0.037
_refine_ls_R_factor_obs          .030
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0478P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.075
_refine_ls_wR_factor_obs         .073
_reflns_number_observed          4449
_reflns_number_total             5056
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            fg1296.cif
_cod_data_source_block           hbn
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 

The following automatic conversions were performed:

'_chemical_melting_point' value '247C' was changed to '520.15' - it
was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '247C' was changed to '520.15' - it
was converted from degrees Celsius(C) to
Kelvins(K).

'_symmetry_cell_setting' value 'Monoclinic' changed to
'monoclinic' 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_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0478P)^2^] where P=(Fo^2^+2Fc^2^)/3' was changed
to 'calc'. New tag '_refine_ls_weighting_details' was created. The
value of the new tag was set to 'w = 1/[\s^2^(Fo^2^)+(0.0478P)^2^]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1674.0(8)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2006577