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_7040373
_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 H37 B19 Ni P2'
_chemical_formula_sum            'C10 H37 B19 Ni P2'
_chemical_formula_weight         483.43
_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
_audit_creation_date             2016-02-09
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-07-12 deposited with the CCDC.
2016-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                112.101(4)
_cell_angle_beta                 97.903(4)
_cell_angle_gamma                99.226(4)
_cell_formula_units_Z            2
_cell_length_a                   9.0457(7)
_cell_length_b                   12.1143(10)
_cell_length_c                   13.0918(11)
_cell_measurement_reflns_used    8122
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.09
_cell_measurement_theta_min      2.63
_cell_volume                     1280.96(19)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.955
_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  0.0328
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21467
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.325
_diffrn_reflns_theta_min         1.720
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.883
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6999
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0548 before and 0.0446 after correction.
The Ratio of minimum to maximum transmission is 0.9387.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.759
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         6101
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0342
_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^)+(0.0348P)^2^+0.9552P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0811
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5257
_reflns_number_total             6101
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02855a2.cif
_cod_data_source_block           x85030
_cod_depositor_comments
'Adding full bibliography for 7040371--7040379.cif.'
_cod_original_cell_volume        1280.96(18)
_cod_database_code               7040373
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.742
_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, All C(H,H,H,H,H,H) groups
2. Shared sites
{C2', B2'}
{C6', B6'}
3. Uiso/Uaniso restraints and constraints
P2 \\sim P2A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C102) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(B2') = Uanis(C2')
Uanis(C6') = Uanis(B6')
4. Others
 Sof(C102)=Sof(H10C)=Sof(H10D)=Sof(C202)=Sof(H20C)=Sof(H20D)=Sof(H21D)=
 Sof(H21E)=Sof(H21F)=Sof(P2A)=1-FVAR(1)
 Sof(P2)=Sof(C101)=Sof(H10A)=Sof(H10B)=Sof(C201)=Sof(H20A)=Sof(H20B)=Sof(H21A)=
 Sof(H21B)=Sof(H21C)=FVAR(1)
 Sof(B2')=Sof(C6')=1-FVAR(2)
 Sof(C2')=Sof(B6')=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C101(H10A,H10B), C102(H10C,H10D), C201(H20A,H20B), C202(H20C,H20D)
5.b Me refined with riding coordinates:
 C211(H21A,H21B,H21C), C211(H21D,H21E,H21F), C221(H22A,H22B,H22C)
5.c Idealised Me refined as rotating group:
 C111(H11A,H11B,H11C), C121(H12A,H12B,H12C)
;
_olex2_submission_special_instructions 'No special instructions were received'