Reversible water activation driven by contraction and expansion of a 12-vertex-closo-12-vertex-nido biscarborane cluster.
Wong, Yuen Onn; Smith, Mark D.; Peryshkov, Dmitry V.; Chemical communications (Cambridge, England) 52 (2016) 12710–12713; doi:10.1039/c6cc06955j

data_7125123
_publ_section_title
;
 Reversible water activation driven by contraction and expansion of a
 12-vertex-closo-12-vertex-nido biscarborane cluster.
;
_journal_issue                   86
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12710
_journal_page_last               12713
_journal_paper_doi               10.1039/c6cc06955j
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C28 H78 B20 N4 O P2, C H2 Cl2'
_chemical_formula_sum            'C29 H80 B20 Cl2 N4 O P2'
_chemical_formula_weight         850.01
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-09-24
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-06-22 deposited with the CCDC.
2016-09-15 downloaded from the CCDC.
;
_cell_angle_alpha                92.3050(10)
_cell_angle_beta                 91.8090(10)
_cell_angle_gamma                98.8840(10)
_cell_formula_units_Z            2
_cell_length_a                   11.8867(4)
_cell_length_b                   12.3732(4)
_cell_length_c                   16.8070(6)
_cell_measurement_reflns_used    9778
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      2.52
_cell_volume                     2438.50(14)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEXII v2014.9-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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(2)
_diffrn_detector                 'Bruker PHOTON-100 area detector'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            126383
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        30.075
_diffrn_reflns_theta_max         30.077
_diffrn_reflns_theta_min         2.155
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.230
_exptl_absorpt_correction_T_max  0.4326
_exptl_absorpt_correction_T_min  0.4009
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0729 before and 0.0505 after correction.
The Ratio of minimum to maximum transmission is 0.9267.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_description       block
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.0049(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         14334
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0351
_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^)+(0.0340P)^2^+1.2061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0846
_reflns_number_gt                12190
_reflns_number_total             14334
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc06955j2.cif
_cod_data_source_block           c1npamino
_cod_database_code               7125123
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.922
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C51-Cl1 \\sim C51-Cl2A \\sim C51-Cl2B
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(Cl2A) = Uanis(Cl2B)
4. Others
 Sof(Cl2B)=Sof(H51C)=Sof(H51D)=1-FVAR(1)
 Sof(Cl2A)=Sof(H51A)=Sof(H51B)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C11(H11A), C14(H14A), C17(H17A), C20(H20A), C31(H31), C34(H34), C37(H37),
 C40(H40)
5.b Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C51(H51C,H51D)
5.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15B,H15C,H15D), C16(H16A,H16B,
 H16C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,
 H22B,H22C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C),
 C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,
 H41C), C42(H42A,H42B,H42C)
;
_shelx_res_checksum              66930
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'