Boratocarbyne Complexes: Li[Mo{≡CB(OMe)3}(CO)2{HB(pzMe2)3}] and [K(18-crown-6)][Mo(≡CBF2OMe)(CO)2{HB(pzMe2)3}] (pz = pyrazol-1-yl)
Hill, Anthony F.; Shang, Rong; Organometallics 31 (2012) 4635–; doi:10.1021/om300238m

data_4078655
_publ_section_title
;
 Boratocarbyne Complexes: Li[Mo{\\tb CB(OMe)3}(CO)2{HB(pzMe2)3}] and
 [K(18-crown-6)][Mo(\\tb CBF2OMe)(CO)2{HB(pzMe2)3}] (pz = pyrazol-1-yl)
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              4635
_journal_paper_doi               10.1021/om300238m
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C37 H55 B2 F2 K1 Mo1 N6 O9'
_chemical_formula_sum            'C37 H55 B2 F2 K Mo N6 O9'
_chemical_formula_weight         922.53
_chemical_name_systematic
; 
 [Tp'(CO)~2~MoCBF~2~(OMe)]K.C~12~H~24~O~6~.C~6~H~6~
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             09-09-07
_audit_creation_method           CRYSTALS_ver_12.85
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.4593(3)
_cell_length_b                   18.6396(2)
_cell_length_c                   25.1695(4)
_cell_measurement_reflns_used    52345
_cell_measurement_temperature    200
_cell_measurement_theta_max      24.4
_cell_measurement_theta_min      2.6
_cell_volume                     9129.3(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  0.064
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            81093
_diffrn_reflns_theta_full        24.473
_diffrn_reflns_theta_max         24.473
_diffrn_reflns_theta_min         2.555
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.441
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.887
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via Gaussian method (Coppens, 1970) implemented in maXus (Mackay et al, 2000)
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3840
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.47
_refine_diff_density_min         -0.62
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9828
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         7532
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0261
_refine_ls_shift/su_max          0.012880
_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: 
 19.2 30.0 15.4 4.14 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1065
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.1065
_reflns_limit_h_max              22
_reflns_limit_h_min              0
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              29
_reflns_limit_l_min              0
_reflns_number_gt                4264
_reflns_number_total             7560
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.84
_oxford_diffrn_Wilson_scale      190.60
_oxford_refine_ls_r_factor_ref   0.0555
_oxford_refine_ls_scale          0.10951(3)
_oxford_reflns_number_all        7532
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title rong025
_cod_data_source_file            om300238m_si_001.cif
_cod_data_source_block           rong025
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P b c a '
_cod_original_formula_sum        'C37 H55 B2 F2 K1 Mo1 N6 O9'
_cod_database_code               4078655