Synthesis of a Thiocarbamoyl Alkylidyne Complex and Caveats Associated with the Use of [Mo(≡CLi)(CO)2(Tp*)] (Tp* = Hydrotris(3,5-dimethylpyrazol-1-yl)borate)
Colebatch, Annie L.; Hill, Anthony F.; Shang, Rong; Willis, Anthony C.; Organometallics 29 (2010) 6482–; doi:10.1021/om1008296

data_4067095
_publ_section_title
;
 Synthesis of a Thiocarbamoyl Alkylidyne Complex and Caveats Associated
 with the Use of [Mo(\\tb CLi)(CO)2(Tp*)] (Tp* =
 Hydrotris(3,5-dimethylpyrazol-1-yl)borate)
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6482
_journal_paper_doi               10.1021/om1008296
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C21 H28 B1 Mo1 N7 O2 S1'
_chemical_formula_sum            'C21 H28 B Mo N7 O2 S'
_chemical_formula_weight         549.32
_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
_audit_creation_date             08-09-17
_audit_creation_method           CRYSTALS_ver_12.85
_audit_update_record
;
2008-06-25 - Report on C~21~H~28~BMoN~7~O~2~S
            by Rong Shang  
            for Anthony F. Hill, Annie L. Colebatch

2008-06-25 - passes checkcif tests with minor warnings

;
_cell_angle_alpha                90
_cell_angle_beta                 107.1193(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2972(3)
_cell_length_b                   17.1306(7)
_cell_length_c                   14.0712(4)
_cell_measurement_reflns_used    14660
_cell_measurement_temperature    200
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.7
_cell_volume                     2602.52(15)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2008)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_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  0.090
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            32448
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         2.745
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.615
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.946
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.56
_refine_diff_density_min         -0.75
_refine_ls_extinction_coef       136(14)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9394
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4594
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.000852
_refine_ls_structure_factor_coef Fsqd
_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: 
 15.1 23.4 12.0 3.24 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1186
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.1186
_reflns_limit_h_max              12
_reflns_limit_h_min              -13
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                2741
_reflns_number_total             4594
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.05
_oxford_diffrn_Wilson_scale      52.63
_oxford_refine_ls_r_factor_ref   0.0645
_oxford_refine_ls_scale          0.14902(10)
_oxford_reflns_number_all        4594
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title '9171147 rong010'
_cod_data_source_file            om1008296_si_001.cif
_cod_data_source_block           Compound_3
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C21 H28 B1 Mo1 N7 O2 S1'
_cod_database_code               4067095