Group 14 Substituted Carbyne Complexes—An Almost Complete Set: [Mo(\τb CAPh3)(CO)2(Tp*)] (Tp* = Hydrotris(dimethylpyrazolyl)borate; A = Si, Ge, Sn, Pb but A ≠ C)
Cordiner, Richard L.; Hill, Anthony F.; Shang, Rong; Willis, Anthony C.; Organometallics 30 (2011) 139–; doi:10.1021/om100896r

data_4063731
_publ_section_title
;
 Group 14 Substituted Carbyne Complexes---An Almost Complete Set: [Mo(\\tb
 CAPh3)(CO)2(Tp*)] (Tp* = Hydrotris(dimethylpyrazolyl)borate; A = Si, Ge,
 Sn, Pb but A =&#x0338; C)
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              139
_journal_paper_doi               10.1021/om100896r
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C36 H37 B1 Mo1 N6 O2 Si1'
_chemical_formula_sum            'C36 H37 B Mo N6 O2 Si'
_chemical_formula_weight         720.57
_chemical_name_systematic
; 
 Tp'(CO)~2~Mo(_-C)SiPh~3~'
;
_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             09-06-22
_audit_creation_method           CRYSTALS_ver_12.85
_cell_angle_alpha                101.4756(11)
_cell_angle_beta                 91.0133(14)
_cell_angle_gamma                95.6878(13)
_cell_formula_units_Z            2
_cell_length_a                   10.3477(2)
_cell_length_b                   12.1245(3)
_cell_length_c                   14.3177(3)
_cell_measurement_reflns_used    17898
_cell_measurement_temperature    200
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      2.55
_cell_volume                     1750.44(7)
_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  0.045
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            31719
_diffrn_reflns_theta_full        26.373
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         2.738
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.450
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.931
_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    1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.49
_refine_diff_density_min         -0.53
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8159
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         7115
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.000784
_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: 
 19.5 28.8 14.3 3.85 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1036
_refine_ls_wR_factor_gt          0.0845
_refine_ls_wR_factor_ref         0.1036
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              14
_reflns_limit_k_min              -15
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                5504
_reflns_number_total             7135
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.22
_oxford_diffrn_Wilson_scale      9.69
_oxford_refine_ls_r_factor_ref   0.0475
_oxford_refine_ls_scale          0.3464(3)
_oxford_reflns_number_all        7115
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title '6221008 rong023'
_cod_data_source_file            om100896r_si_001.cif
_cod_data_source_block           Compound_2
_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 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C36 H37 B1 Mo1 N6 O2 Si1'
_cod_database_code               4063731