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_7040372
_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
'C30 H45 B19 Ni P2, 0.5(C H2 Cl2), C0.25 H0.99 Cl0.99, 0.25(C1)'
_chemical_formula_sum            'C31 H47 B19 Cl2 Ni P2'
_chemical_formula_weight         816.62
_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             2015-07-17
_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                70.135(4)
_cell_angle_beta                 74.434(4)
_cell_angle_gamma                74.312(4)
_cell_formula_units_Z            2
_cell_length_a                   10.2951(8)
_cell_length_b                   13.7359(10)
_cell_length_c                   16.4159(13)
_cell_measurement_reflns_used    9987
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      33.52
_cell_measurement_theta_min      2.69
_cell_volume                     2061.6(3)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_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  0.0417
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            59426
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         33.989
_diffrn_reflns_theta_min         2.701
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.704
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.6817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0594 before and 0.0489 after correction.
The Ratio of minimum to maximum transmission is 0.9130.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.234
_refine_diff_density_min         -0.885
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         16558
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0455P)^2^+0.9777P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1089
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12922
_reflns_number_total             16558
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02855a2.cif
_cod_data_source_block           5029
_cod_depositor_comments
'Adding full bibliography for 7040371--7040379.cif.'
_cod_database_code               7040372
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.747
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
2. Shared sites
{C2S, Cl2S}
{C3S, Cl3S}
3. Uiso/Uaniso restraints and constraints
Uanis(C3S) = Uanis(Cl3S)
Uanis(C3S) = Uanis(C3T)
Uanis(C2S) = Uanis(Cl2S)
4. Others
 Sof(Cl2S)=Sof(H3SA)=Sof(H3SB)=Sof(Cl4S)=1-FVAR(1)
 Sof(C3S)=Sof(C3T)=0.5*(1-FVAR(2))
 Sof(Cl1S)=Sof(C2S)=Sof(H2SA)=Sof(H2SB)=Sof(Cl3S)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C101(H10A,H10B), C201(H20A,H20B), C2S(H2SA,H2SB), C3S(H3SA,H3SB)
5.b Aromatic/amide H refined with riding coordinates:
 C112(H112), C113(H113), C114(H114), C115(H115), C116(H116), C122(H122),
 C123(H123), C124(H124), C125(H125), C126(H126), C212(H212), C213(H213),
 C214(H214), C215(H215), C216(H216), C222(H222), C223(H223), C224(H224),
 C225(H225), C226(H226)
;
_olex2_submission_special_instructions 'No special instructions were received'