A tetranuclear arylstibonic acid with an adamantane type structure.
Brünig, Julian; Hupf, Emanuel; Lork, Enno; Mebs, Stefan; Beckmann, Jens; Dalton transactions (Cambridge, England : 2003) 44 (2015) 7105–7108; doi:10.1039/c5dt00588d

data_7034398
_publ_section_title
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 A tetranuclear arylstibonic acid with an adamantane type structure.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7105
_journal_page_last               7108
_journal_paper_doi               10.1039/c5dt00588d
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C96 H76 O10 P4 Sb4, 4(C H2 Cl2)'
_chemical_formula_sum            'C100 H84 Cl8 O10 P4 Sb4'
_chemical_formula_weight         2340.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-02-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-03-10 deposited with the CCDC.
2015-03-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.7330(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.2249(10)
_cell_length_b                   20.2061(9)
_cell_length_c                   26.9813(13)
_cell_measurement_reflns_used    8609
_cell_measurement_temperature    173.01
_cell_measurement_theta_max      23.79
_cell_measurement_theta_min      2.37
_cell_volume                     10958.5(9)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_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  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.01
_diffrn_detector                 'Bruker PHOTON area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture CMOS'
_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  0.2083
_diffrn_reflns_av_unetI/netI     0.1352
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            81463
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.498
_diffrn_reflns_theta_min         2.371
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.280
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6432
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.0802 before and 0.0681 after correction.
The Ratio of minimum to maximum transmission is 0.8627.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_description       block
_exptl_crystal_F_000             4656
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.709
_refine_diff_density_min         -1.240
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     616
_refine_ls_number_reflns         10206
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1078
_refine_ls_R_factor_gt           0.0631
_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^)+(0.0838P)^2^+50.1208P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1559
_refine_ls_wR_factor_ref         0.1698
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6686
_reflns_number_total             10206
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00588d2.cif
_cod_data_source_block           bruening140731_0m
_cod_depositor_comments
'Adding full bibliography for 7034397--7034398.cif.'
_cod_database_code               7034398
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 C33'-C32'
 1.4 with sigma of 0.02
 C34'-C35'
 1.4 with sigma of 0.02
 C30-C35
 1.4 with sigma of 0.02
 C34-C33
 1.4 with sigma of 0.02
 C34-C33
 1.4 with sigma of 0.02
 C30-C35
 1.4 with sigma of 0.02
 C34-C35
 1.4 with sigma of 0.02
 C30-C31'
 1.4 with sigma of 0.02
 C35'-C30
 1.4 with sigma of 0.02
 C31'-C30
 1.4 with sigma of 0.02
3. Restrained planarity
 C30, C31, C32, C33, C34, C35
 with sigma of 0.1
 C30, C31', C32', C33', C34', C35'
 with sigma of 0.1
4. Rigid body (RIGU) restrains
 C31', C32', C33', C34', C35'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C30, C31, C32, C33, C34, C35
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C30, C31, C32, C33, C34, C35
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C31(0.7) H31(0.7) C32(0.7) H32(0.7) C33(0.7) H33(0.7) C34(0.7)
 H34(0.7) C35(0.7) H35(0.7) C31'(0.3) H31'(0.3) C32'(0.3) H32'(0.3) C33'(0.3)
 H33'(0.3) C34'(0.3) H34'(0.3) C35'(0.3) H35'(0.3)
6.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C1(H1A,H1B), C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B), C5(H5A,H5B)
6.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C16(H16), C17(H17), C21(H21), C22(H22), C23(H23),
 C24(H24), C25(H25), C41(H41), C42(H42), C46(H46), C47(H47), C51(H51), C52(H52),
  C53(H53), C54(H54), C55(H55), C61(H61), C62(H62), C63(H63), C64(H64),
 C65(H65), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C31'(H31'),
 C32'(H32'), C33'(H33'), C34'(H34'), C35'(H35')
6.c Idealised tetrahedral OH refined as rotating group:
 O5(H5), O6(H6)
;
_smtbx_masks_special_details
'The unit cell contains 4 more molecules of CH2Cl2 which have been treated as a diffuse contribution to the overall scattering'
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'