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_7040377
_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         'C12 H32 B19 P'
_chemical_formula_sum            'C12 H32 B19 P'
_chemical_formula_weight         412.73
_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             2015-07-23
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2016-07-12 deposited with the CCDC.
2016-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.459(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.0021(9)
_cell_length_b                   12.7125(16)
_cell_length_c                   26.754(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      0.000
_cell_measurement_theta_min      0.000
_cell_volume                     2370.7(5)
_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 0.985
_diffrn_measured_fraction_theta_max 0.979
_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  0.0548
_diffrn_reflns_av_unetI/netI     0.0769
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            15432
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.278
_diffrn_reflns_theta_min         2.798
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.117
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6991
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0668 before and 0.0556 after correction.
The Ratio of minimum to maximum transmission is 0.9375.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_description       plate
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.576
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.059
_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     355
_refine_ls_number_reflns         5764
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0587
_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^)+(0.0610P)^2^+0.9413P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1334
_refine_ls_wR_factor_ref         0.1481
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4140
_reflns_number_total             5764
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02855a2.cif
_cod_data_source_block           5114
_cod_depositor_comments
'Adding full bibliography for 7040371--7040379.cif.'
_cod_database_code               7040377
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1(0.027) H2(0.026) H3(0.027) H4(0.025) H5(0.024) H6(0.023)
 H8(0.024) H9A(0.023) H9B(0.021) H11(0.03) H10A(0.041) H10B(0.041) H10C(0.041)
 H10D(0.035) H10E(0.035) H10F(0.035) H104(0.029) H105(0.036) H106(0.037)
 H107(0.035) H108(0.03) H2'(0.036) H3'(0.027) H4'(0.025) H5'(0.022) H6'(0.024)
 H7'(0.03) H9'(0.028) H10'(0.027) H11'(0.03) H12'(0.031)
 Fixed X: H10A(0.0484) H10B(0.1892) H10C(0.1233) H10D(0.5092) H10E(0.5748)
 H10F(0.6647) H104(0.5495) H105(0.4786) H106(0.1928) H107(-0.0286) H108(0.0416)
 Fixed Y: H10A(0.5592) H10B(0.632) H10C(0.6685) H10D(0.6959) H10E(0.6636)
 H10F(0.6048) H104(0.5541) H105(0.4926) H106(0.4034) H107(0.38) H108(0.4385)
 Fixed Z: H10A(0.1743) H10B(0.1456) H10C(0.1986) H10D(0.238) H10E(0.1844)
 H10F(0.234) H104(0.3107) H105(0.3887) H106(0.3966) H107(0.327) H108(0.2481)
;
_olex2_submission_special_instructions 'No special instructions were received'