Steric versus electronic factors in metallacarborane isomerisation: nickelacarboranes with 3,1,2-, 4,1,2- and 2,1,8-NiC2B9 architectures and pendant carborane groups, derived from 1,1'-bis(o-carborane).
Mandal, Dipendu; Man, Wing Y.; Rosair, Georgina M.; Welch, Alan J.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 15013–15025; doi:10.1039/c6dt02855a

data_7040378
_publ_section_title
;
 Steric versus electronic factors in metallacarborane isomerisation:
 nickelacarboranes with 3,1,2-, 4,1,2- and 2,1,8-NiC2B9 architectures and
 pendant carborane groups, derived from 1,1'-bis(o-carborane).
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15013
_journal_page_last               15025
_journal_paper_doi               10.1039/c6dt02855a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C10 H39 B19 Ni O6 P2'
_chemical_formula_sum            'C10 H39 B19 Ni O6 P2'
_chemical_formula_weight         581.45
_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             2016-02-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-07-12 deposited with the CCDC.
2016-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                109.302(4)
_cell_angle_beta                 95.518(5)
_cell_angle_gamma                93.573(6)
_cell_formula_units_Z            2
_cell_length_a                   11.0321(11)
_cell_length_b                   11.6703(12)
_cell_length_c                   11.8503(11)
_cell_measurement_reflns_used    1738
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.395
_cell_measurement_theta_min      2.449
_cell_volume                     1426.1(2)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.960
_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     0.0666
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5415
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.045
_diffrn_reflns_theta_min         2.761
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.820
_exptl_absorpt_correction_T_max  0.745314
_exptl_absorpt_correction_T_min  0.556700
_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 0.0645 before and 0.0516 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 0.1127 before and 0.0678 after correction.
 The Ratio of minimum to maximum transmission is 0.75.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 28465 reflections, Rint = 0.0850
 (11666 with I > 3sig(I), Rint = 0.0727)
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         5415
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.001
_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^+0.3624P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1106
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4117
_reflns_number_total             5415
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02855a2.cif
_cod_data_source_block           5420
_cod_depositor_comments
'Adding full bibliography for 7040371--7040379.cif.'
_cod_database_code               7040378
_shelx_estimated_absorpt_t_max   0.937
_shelx_estimated_absorpt_t_min   0.757
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.835(5) 0.165(5)
2. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'