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_7037969
_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         'C4 H20 B20 N2 O2'
_chemical_formula_sum            'C4 H20 B20 N2 O2'
_chemical_formula_weight         344.42
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n'
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_atom_sites_solution_hydrogens   difmap
_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            4
_cell_length_a                   16.3052(5)
_cell_length_b                   16.3052(5)
_cell_length_c                   6.9144(3)
_cell_measurement_reflns_used    9251
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      28.853
_cell_measurement_theta_min      2.498
_cell_volume                     1838.26(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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0433
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            37192
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.613
_diffrn_reflns_theta_min         1.249
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0586 before and 0.0532 after correction.
The Ratio of minimum to maximum transmission is 0.9177.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_description       block
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         2593
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0693P)^2^+0.1814P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1160
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2457
_reflns_number_total             2593
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04831a1.cif
_cod_data_source_block           4807f
_cod_depositor_comments
'Adding full bibliography for 7037966--7037977.cif.'
_cod_original_cell_volume        1838.26(14)
_cod_database_code               7037969
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.980
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.4665(18) 0.5335(18)
2. Fixed Uiso
 At 1.2 times of:
  All B(H) groups
3. Uiso/Uaniso restraints and constraints
O73 \\sim O74 \\sim O75 \\sim O72: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(O74) \\sim Ueq, Uanis(O75) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O72) = Uanis(O73)
Uanis(O74) = Uanis(O75)
4. Others
 1*[Sof(O72)]+1*[Sof(O74)]+1*[Sof(O75)]+1*[Sof(O73)]=1 with esd of 0.001
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'