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_7037968
_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         'C8 H15 B10 N O'
_chemical_formula_sum            'C8 H15 B10 N O'
_chemical_formula_weight         249.31
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_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             2015-10-13
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.009(2)
_cell_length_b                   15.970(4)
_cell_length_c                   22.139(6)
_cell_measurement_reflns_used    320
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      13.98
_cell_measurement_theta_min      2.71
_cell_volume                     2831.7(13)
_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      150.15
_diffrn_measured_fraction_theta_full 0.968
_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_unetI/netI     0.1752
_diffrn_reflns_laue_measured_fraction_full 0.968
_diffrn_reflns_laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3783
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        22.073
_diffrn_reflns_theta_max         22.073
_diffrn_reflns_theta_min         1.840
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2008/4 (Bruker,2010) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1231 before and 0.0818 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1525 before and 0.0608 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 3:
 wR2(int) was 0.1347 before and 0.0595 after correction.
 The Ratio of minimum to maximum transmission is 0.66.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 21512 reflections, Rint = 0.1327
 (3915 with I > 3sig(I), Rint = 0.0900)
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_description       plate
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.285
_refine_diff_density_min         -0.210
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         3783
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.2405
_refine_ls_R_factor_gt           0.1302
_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^)+(0.1696P)^2^+2.5548P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3038
_refine_ls_wR_factor_ref         0.3858
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1858
_reflns_number_total             3783
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04831a1.cif
_cod_data_source_block           4840
_cod_depositor_comments
'Adding full bibliography for 7037966--7037977.cif.'
_cod_database_code               7037968
_shelx_estimated_absorpt_t_max   0.998
_shelx_estimated_absorpt_t_min   0.979
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.641(10) 0.269(7) 0.090(7)
2. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All B(H,H) groups, All C(H) groups
3. Shared sites
{C1, B1}
{B10, C10}
4. Restrained distances
 N10-C10 \\sim N1-C1
 with sigma of 0.02
 O10-N10 \\sim O1-N1
 with sigma of 0.02
 C10-O10 \\sim C1-O1
 with sigma of 0.02
5. Uiso/Uaniso restraints and constraints
B10 \\sim B5: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C1) = Uanis(B1)
Uanis(C10) = Uanis(B10)
6. Others
 Sof(H2B)=Sof(H3B)=Sof(H4B)=Sof(H5B)=Sof(H6B)=Sof(H9B)=Sof(O10)=Sof(N10)=
 Sof(H11A)=Sof(H12A)=Sof(C10)=Sof(B1)=Sof(H1)=1-FVAR(1)
 Sof(C1)=Sof(N1)=Sof(O1)=Sof(H2A)=Sof(H3A)=Sof(H4A)=Sof(H5A)=Sof(H6A)=Sof(H9A)=
 Sof(B10)=Sof(H10)=Sof(H11)=Sof(H12)=FVAR(1)
7.a Aromatic/amide H refined with riding coordinates:
 C72(H72), C73(H73), C74(H74), C75(H75), C76(H76)
7.b Boron cage BH refined with riding coordinates:
 B2(H2A), B2(H2B), B3(H3A), B3(H3B), B4(H4A), B4(H4B), B5(H5A), B5(H5B),
 B6(H6A), B6(H6B), B8(H8), B9(H9A), B9(H9B), B10(H10), B11(H11), B11(H11A),
 B12(H12), B12(H12A), B1(H1)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'