Trioxorhena(VII)carborane Anion and Its Methyl-Substituted Analogue: Synthesis, Structure, DFT, and Catalytic Studies
Pichaandi, Kothanda Rama; Fanwick, Phillip E.; Abu-Omar, Mahdi M.; Organometallics 31 (2012) 1888–; doi:10.1021/om201222r

data_4076457
_publ_section_title
;
 Trioxorhena(VII)carborane Anion and Its Methyl-Substituted Analogue:
 Synthesis, Structure, DFT, and Catalytic Studies
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1888
_journal_paper_doi               10.1021/om201222r
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C4 H15 B9 O3 Re1,C16 H36 N1'
_chemical_formula_sum            'C20 H51 B9 N O3 Re'
_chemical_formula_weight         637.13
_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_type_scat_source
'International Tables for Crystallography (Vol C)'
_cell_angle_alpha                90.00
_cell_angle_beta                 95.052(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.3733(10)
_cell_length_b                   11.3361(7)
_cell_length_c                   19.5318(14)
_cell_measurement_reflns_used    4660
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      63
_cell_measurement_theta_min      2
_cell_volume                     3170.1(4)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'
_computing_data_collection       'CrystalClear(Rigaku, 2001)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'
_computing_molecular_graphics
;
    ORTEP (Johnson, 1976)
    PLATON (Spek, 2003)
;
_computing_publication_material  'SHELX97(Sheldrick, 2008) and local programs'
_computing_structure_refinement  'SHELX97 (Sheldrick, 2008)'
_computing_structure_solution
;
 PATTY (DIRDIF, Beurskins, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.9690
_diffrn_measured_fraction_theta_max 0.9690
_diffrn_measurement_details
;
Data were collected on a Rigaku Rapid which has a quarter 
chi circle and a 200 degree curved image plate at a fixed 
distance of 127.4mm.  Strategy was optimized using the 
CrystalClear software.  The completeness is the best 
that can be obtained with this geometry. The missing data are not cusp 
data but mostly high angle data.
Also the use of HKL2000/SCALEPACK lowers the number 
of observed data as inconsistent equivalents are removed 
from the data set and not included in the collected total
;
_diffrn_measurement_device_type  Rigaku_Rapid_II
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'confocal optics'
_diffrn_radiation_type           CU-K\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0750
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23105
_diffrn_reflns_theta_full        56.0
_diffrn_reflns_theta_max         63.38
_diffrn_reflns_theta_min         2.27
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.633
_exptl_absorpt_correction_T_max  0.7953
_exptl_absorpt_correction_T_min  0.6071
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.27
_refine_diff_density_min         -0.42
_refine_ls_d_res_high            0.93
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         3998
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.078
_refine_ls_R_factor_gt           0.063
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1396P)^2^+1.2112P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.194
_refine_ls_wR_factor_ref         0.213
_reflns_number_gt                2874
_reflns_number_total             3998
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            om201222r_si_004.cif
_cod_data_source_block           RAM111
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc ' changed to 'calc'
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 

The following automatic conversions were performed:

data name '_iucr_refine_instruction_details' was replaced with
'_iucr_refine_instructions_details' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
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_cod_original_formula_sum        'C20 H51 B9 N1 O3 Re1'
_cod_database_code               4076457