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_7040376
_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         'C20 H43 B19 Ni P2'
_chemical_formula_sum            'C20 H43 B19 Ni P2'
_chemical_formula_weight         609.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-15
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-07-19 deposited with the CCDC.
2016-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.703(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.8159(13)
_cell_length_b                   11.0792(15)
_cell_length_c                   14.558(2)
_cell_measurement_reflns_used    1238
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      16.179
_cell_measurement_theta_min      2.310
_cell_volume                     1583.1(4)
_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  'XH (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.1330
_diffrn_reflns_av_unetI/netI     0.1580
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17876
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        24.825
_diffrn_reflns_theta_max         24.825
_diffrn_reflns_theta_min         2.310
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.729
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1204 before and 0.1009 after correction.
The Ratio of minimum to maximum transmission is 0.6578.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.526
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.44(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         4833
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1216
_refine_ls_R_factor_gt           0.0699
_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^)+(0.0618P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1353
_refine_ls_wR_factor_ref         0.1567
_reflns_Friedel_coverage         0.892
_reflns_Friedel_fraction_full    0.987
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                3249
_reflns_number_total             4833
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02855a2.cif
_cod_data_source_block           5106
_cod_depositor_comments
'Adding full bibliography for 7040371--7040379.cif.'
_cod_database_code               7040376
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.856
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.56(4) 0.44(4)
2. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All B(H,H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Shared sites
{B4, C4}
{C2, B2}
4. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.02
Uanis(B4) = Uanis(C4)
Uanis(C2) = Uanis(B2)
5. Others
 Fixed Sof: B2(0.15) C2(0.85) B4(0.85) C4(0.15) H11A(0.15) H11(0.85)
6.a Aromatic/amide H refined with riding coordinates:
 C104(H104), C105(H105), C106(H106), C107(H107), C108(H108), C204(H204),
 C205(H205), C206(H206), C207(H207), C208(H208)
6.b Idealised Me refined as rotating group:
 C101(H10A,H10B,H10C), C102(H10D,H10E,H10F), C201(H20A,H20B,H20C), C202(H20D,
 H20E,H20F)
6.c Boron cage BH refined with riding coordinates:
 B11(H11A), B11(H11), C2'(H2')
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'