Poly(methimazolyl)borato Nitrosyl Complexes of Molybdenum and Tungsten
Abernethy, Robyn J.; Foreman, Mark R. St.-J.; Hill, Anthony F.; Tshabang, Never; Willis, Anthony C.; Young, Rowan D.; Organometallics 27 (2008) 4455–; doi:10.1021/om800416j

data_4071839
_publ_section_title
;
 Poly(methimazolyl)borato Nitrosyl Complexes of Molybdenum and Tungsten
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4455
_journal_paper_doi               10.1021/om800416j
_journal_volume                  27
_journal_year                    2008
_chemical_compound_source        local
_chemical_formula_moiety         'C28 H27 B N5 O3 P S2 W, C H2 Cl2'
_chemical_formula_sum            'C29 H29 B Cl2 N5 O3 P S2 W'
_chemical_formula_weight         856.25
_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
_audit_creation_date             08-04-18
_audit_creation_method           CRYSTALS_ver_12.18
_audit_update_record
;
2003-04-08    - data collected and early structure done
2008-04-16  - pick up and finish off
2008-04-22 - Report on C29 H29 B Cl2 N5 O3 P S2 W 
            by Anthony C. Willis
            for   Anthony F. Hill and Never Tshabang

2008-04-22 - passes checkcif tests with minor warnings

;
_cell_angle_alpha                95.5217(14)
_cell_angle_beta                 90.9341(12)
_cell_angle_gamma                102.7447(19)
_cell_formula_units_Z            2
_cell_length_a                   10.0313(4)
_cell_length_b                   10.3673(4)
_cell_length_c                   16.8936(7)
_cell_measurement_reflns_used    221106
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     1704.38(12)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius BV, 1997)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
; 
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;
_computing_publication_material  'CRYSTALS (Watkin et al 2003)'
_computing_structure_refinement  'CRYSTALS (Watkin et al 2003)'
_computing_structure_solution    'SIR92 (Altomare et al, 1994)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       ' \f and \w scans with CCD '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.057
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29255
_diffrn_reflns_theta_full        25.190
_diffrn_reflns_theta_max         27.681
_diffrn_reflns_theta_min         2.561
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.753
_exptl_absorpt_correction_T_max  0.773
_exptl_absorpt_correction_T_min  0.463
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via Gaussian method (Coppens, 1970) implemented in maXus (Mackay et al, 2000)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             844.
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.28
_refine_diff_density_min         -1.41
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1013
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         5587
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.000599
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, 
(Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 1.02 -0.217 0.623 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0372
_refine_ls_wR_factor_gt          0.0372
_refine_ls_wR_factor_ref         0.0372
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              13
_reflns_limit_k_min              -13
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                5587
_reflns_number_total             7767
_reflns_threshold_expression     I>3.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.2985(3)
_oxford_structure_analysis_title '4091604 nvt3'
_cod_data_source_file            om800416j-file003.cif
_cod_data_source_block           nvt3
_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_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4071839