Metallaboratranes: Bis- and Tris(methimazolyl)borane Complexes of Group 9 Metal Carbonyls and Thiocarbonyls
Crossley, Ian R.; Hill, Anthony F.; Willis, Anthony C.; Organometallics 29 (2010) 326–; doi:10.1021/om900655k

data_4063424
_publ_contact_author_address
;
Research School of Chemistry,
Australian National University,
Canberra, A. C. T. 0200, Australia
;
_publ_contact_author_email       ' willis@rsc.anu.edu.au '
_publ_contact_author_fax         ' 61 2 6125 0750 '
_publ_contact_author_name        ' Anthony C. Willis '
_publ_contact_author_phone       ' 61 2 6125 4109 '
_publ_section_title
;
 Metallaboratranes: Bis- and Tris(methimazolyl)borane Complexes of Group 9
 Metal Carbonyls and Thiocarbonyls
;
_journal_coeditor_notes
;                                                                               
                                  ?                                             
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              326
_journal_paper_doi               10.1021/om900655k
_journal_techeditor_notes
;                                                                               
                                  ?                                             
;
_journal_volume                  29
_journal_year                    2010
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C31 H31 B Ir N6 O P S3, 1.34(C H2 Cl2) '
_chemical_formula_sum            'C32.34 H33.68 B Cl2.68 Ir N6 O P S3'
_chemical_formula_weight         947.36
_chemical_name_systematic
; 
? 
;
_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             05-25-02
_audit_creation_method           CRYSTALS_ver_12-03-99
_audit_update_record
;
2005-02-26 - Report on  C31 H31 B Ir N6 O P S3, 1.34(C H2 Cl2)
             by Anthony C. Willis
             for   Anthony F. Hill and Ian Crossley

2005-03-09 - passes checkcif tests with minor warnings

;
_cell_angle_alpha                90
_cell_angle_beta                 99.9747(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   39.7468(7)
_cell_length_b                   9.6094(1)
_cell_length_c                   20.3913(4)
_cell_measurement_reflns_used    92362
_cell_measurement_temperature    200
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     7670.6(2)
_computing_cell_refinement
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_computing_data_collection
; 
 COLLECT (Nonius BV, 1997) 
;
_computing_data_reduction
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
; 
Nonius Kappa CCD 
;
_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  0.09
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            56225
_diffrn_reflns_theta_full        25.024
_diffrn_reflns_theta_max         25.024
_diffrn_reflns_theta_min         2.632
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.908
_exptl_absorpt_correction_T_max  0.866
_exptl_absorpt_correction_T_min  0.555
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
_exptl_crystal_colour            ' colourless '
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_density_meas      ?
_exptl_crystal_description       ' needle '
_exptl_crystal_F_000             3745.142
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.58
_refine_diff_density_min         -1.10
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0880
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         4591
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0288
_refine_ls_shift/su_max          0.004579
_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: 
 0.957 -0.0516 0.864 -0.0535 0.170 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0353
_refine_ls_wR_factor_gt          0.0315
_refine_ls_wR_factor_ref         0.0315
_reflns_limit_h_max              46
_reflns_limit_h_min              -47
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                4591
_reflns_number_total             6772
_reflns_threshold_expression     I>3.0u(I)
_cod_data_source_file            om900655k_si_002.cif
_cod_data_source_block           irc08
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1673 2011-04-08 12:14:43Z 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      'C 1 2/c 1 '
_cod_original_formula_sum        ' C32.34 H33.68 B Cl2.68 Ir N6 O P S3 '
_cod_database_code               4063424