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_7037976
_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         'C16 H36 B20 N2 O2'
_chemical_formula_sum            'C16 H36 B20 N2 O2'
_chemical_formula_weight         504.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_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                 99.648(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.1193(7)
_cell_length_b                   10.6700(7)
_cell_length_c                   12.4753(8)
_cell_measurement_reflns_used    5528
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      27.006
_cell_measurement_theta_min      2.404
_cell_volume                     1327.94(15)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.984
_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  0.0503
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_laue_measured_fraction_full 0.989
_diffrn_reflns_laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19862
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.162
_diffrn_reflns_theta_min         2.404
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6401
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0780 before and 0.0662 after correction.
The Ratio of minimum to maximum transmission is 0.8586.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_description       block
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.482
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         2902
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.251
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0570
_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^)+(0.0547P)^2^+1.1822P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1325
_refine_ls_wR_factor_ref         0.1442
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2254
_reflns_number_total             2902
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04831a1.cif
_cod_data_source_block           5223
_cod_depositor_comments
'Adding full bibliography for 7037966--7037977.cif.'
_cod_database_code               7037976
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.965
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 O2B-C3B = O1-C3
 1.45 with sigma of 0.02
 C7-C8 \\sim C7B-C4
 with sigma of 0.02
 C3B-C4 \\sim C7B-C6B \\sim C5B-C6B \\sim C3-C8 \\sim C3-C4 \\sim C4-C5 \\sim
C7-C6 \\sim C5-C6
 with sigma of 0.02
3. Others
 Sof(H4AA)=Sof(H4AB)=Sof(H7A)=Sof(O2B)=Sof(C3B)=Sof(H3B)=Sof(C5B)=Sof(H5BA)=
 Sof(C6B)=Sof(H6B)=Sof(C7B)=Sof(H7BA)=Sof(H7BB)=1-FVAR(1)
 Sof(O1)=Sof(C3)=Sof(H3A)=Sof(H4BC)=Sof(H4BD)=Sof(C5)=Sof(H5A)=Sof(H5B)=
 Sof(C6)=Sof(H6A)=Sof(H7B)=Sof(C8)=Sof(H8A)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C3(H3A), C6(H6A), C3B(H3B), C6B(H6B)
4.b Secondary CH2 refined with riding coordinates:
 C4(H4AA,H4AB), C4(H4BC,H4BD), C5(H5A,H5B), C7B(H7BA,H7BB)
4.c Aromatic/amide H refined with riding coordinates:
 C7(H7A), C7(H7B), C8(H8A), C5B(H5BA)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'