Developing nitrosocarborane chemistry.
Powley, Samuel L.; Schaefer, Louise; Man, Wing Y.; Ellis, David; Rosair, Georgina M.; Welch, Alan J.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 3635–3647; doi:10.1039/c5dt04831a

data_7037973
_publ_section_title
;
 Developing nitrosocarborane chemistry.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3635
_journal_page_last               3647
_journal_paper_doi               10.1039/c5dt04831a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C12 H27 B10 N O'
_chemical_formula_sum            'C12 H27 B10 N O'
_chemical_formula_weight         309.44
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-10-07
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-12-03 deposited with the CCDC.
2016-01-12 downloaded from the CCDC.
;
_cell_angle_alpha                87.624(6)
_cell_angle_beta                 88.802(5)
_cell_angle_gamma                71.721(5)
_cell_formula_units_Z            8
_cell_length_a                   11.9847(18)
_cell_length_b                   16.213(3)
_cell_length_c                   20.179(3)
_cell_measurement_reflns_used    6820
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      26.379
_cell_measurement_theta_min      2.374
_cell_volume                     3719.8(11)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0705
_diffrn_reflns_laue_measured_fraction_full 0.981
_diffrn_reflns_laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            30882
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.467
_diffrn_reflns_theta_min         2.456
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.059
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0577 before and 0.0462 after correction.
The Ratio of minimum to maximum transmission is 0.9003.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.105
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.210
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1009
_refine_ls_number_reflns         14855
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0538P)^2^+0.0295P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1175
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10171
_reflns_number_total             14855
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04831a1.cif
_cod_data_source_block           5214
_cod_depositor_comments
'Adding full bibliography for 7037966--7037977.cif.'
_cod_original_cell_volume        3719.8(10)
_cod_database_code               7037973
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.972
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C10C(H10A), C10A(H10G), C10D(H10E), C10B(H10B)
2.b Secondary CH2 refined with riding coordinates:
 C4C(H4CA,H4CB), C5C(H5CA,H5CB), C5D(H5DA,H5DB), C4A(H4AA,H4AB), C4D(H4DA,
 H4DB), C5A(H5AA,H5AB), C4B(H4BA,H4BB), C5B(H5BA,H5BB)
2.c Aromatic/amide H refined with riding coordinates:
 C7C(H7CA), C8C(H8CA), C8B(H8B), C8D(H8D), C8A(H8A), C7A(H7A), C7B(H7B),
 C7D(H7D)
2.d Idealised Me refined as rotating group:
 C9C(H9CA,H9CB,H9CC), C11C(H11A,H11B,H11D), C12C(H12A,H12B,H12D), C11D(H11I,
 H11J,H11K), C12A(H12M,H12N,H12O), C12D(H12I,H12J,H12K), C9A(H9AA,H9AB,H9AC),
 C11A(H11M,H11N,H11O), C9B(H9BA,H9BB,H9BC), C12B(H12E,H12F,H12G), C11B(H11E,
 H11F,H11G), C9D(H9DA,H9DB,H9DC)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'