Alkyne coupling in rhenacarbaborane chemistry. Structure of [1,2-µ-NHBut-2,2-(CO)2-3,2-σ:η2-{C(CHBut)‒CHCHBut}-closo-2,1-ReCB10H9]
Du, Shaowu; Kautz, Jason A.; McGrath, Thomas D.; Stone, F. Gordon A.; Chemical Communications  (2002) 1004–; doi:10.1039/b201772p

data_7114522
_publ_section_title
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 Alkyne coupling in rhenacarbaborane chemistry. Structure of
 [1,2-&#x00B5;-NHBut-2,2-(CO)2-3,2-\s:\h2-{C(&#xE001;CHBut)--CH&#xE001;CHBut}-closo-2,1-ReCB10H9]
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_journal_issue                   9
_journal_name_full               'Chemical Communications'
_journal_page_first              1004
_journal_paper_doi               10.1039/b201772p
_journal_year                    2002
_chemical_formula_sum            'C19 H40 B10 N O2 Re'
_chemical_formula_weight         608.82
_chemical_name_systematic
; 
? 
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2001
_audit_creation_method           SHELX-97
_audit_update_record
;
?
;
_cell_angle_alpha                90.00
_cell_angle_beta                 92.828(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.4396(16)
_cell_length_b                   15.369(2)
_cell_length_c                   15.377(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      15
_cell_volume                     2700.2(6)
_computing_cell_refinement       'Enraf-Nonius CAD4 (1989)'
_computing_data_collection       'Enraf-Nonius CAD4 (1989)'
_computing_data_reduction        'XCAD4 Siemens Software (Harms, 1993)'
_computing_molecular_graphics    'XP in SHELXTL-PC (Bruker, 1995)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w-5/3\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_sigmaI/netI    0.0608
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5032
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         1.87
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.517
_exptl_absorpt_correction_T_max  0.5545
_exptl_absorpt_correction_T_min  0.3056
_exptl_absorpt_correction_type   'Empirical, \y-scan'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.316
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         4777
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0314P)^2^+1.5584P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0715
_refine_ls_wR_factor_ref         0.0808
_reflns_number_gt                3448
_reflns_number_total             4777
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b201772p.txt
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0314P)^2^+1.5584P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0314P)^2^+1.5584P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2700.2(7)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7114522