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_4067097
_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         'C36 H46 B2 Mo2 N12 O4, 1.5(C6 H14)'
_chemical_formula_sum            'C45 H67 B2 Mo2 N12 O4'
_chemical_formula_weight         1053.61
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             08-07-07
_audit_creation_method           CRYSTALS_ver_12.85
_audit_update_record
;

2010-07-30 - acw edits cif

;
_cell_angle_alpha                90
_cell_angle_beta                 101.4488(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.5979(3)
_cell_length_b                   25.1666(3)
_cell_length_c                   17.0814(2)
_cell_measurement_reflns_used    89945
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     10363.8(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.056
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            98357
_diffrn_reflns_theta_full        27.499
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.571
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.536
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.803
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Via Gaussian method (Coppens, 1970) implemented in maXus (Mackay et al, 2000)
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4376
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.68
_refine_diff_density_min         -0.57
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9828
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         11838
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.007989
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 6.46P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1087
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1087
_reflns_limit_h_max              31
_reflns_limit_h_min              -31
_reflns_limit_k_max              32
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                8588
_reflns_number_total             11871
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.52
_oxford_diffrn_Wilson_scale      88.35
_oxford_refine_ls_r_factor_ref   0.0573
_oxford_refine_ls_scale          0.11804(3)
_oxford_reflns_number_all        11838
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title '7021622 rong002'
_cod_data_source_file            om1008296_si_001.cif
_cod_data_source_block           Compound_5a_Hexane_solvate
_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      'C 1 2/c 1 '
_cod_database_code               4067097