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_7034397
_publ_section_title
;
 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         'C24 H18 Cl4 P Sb, C4 H8 O'
_chemical_formula_sum            'C28 H26 Cl4 O P Sb'
_chemical_formula_weight         673.01
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-02-26
_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                101.464(2)
_cell_angle_beta                 106.588(2)
_cell_angle_gamma                90.666(2)
_cell_formula_units_Z            2
_cell_length_a                   9.6541(5)
_cell_length_b                   10.0084(5)
_cell_length_c                   16.5724(8)
_cell_measurement_reflns_used    9533
_cell_measurement_temperature    173
_cell_measurement_theta_max      32.52
_cell_measurement_theta_min      2.62
_cell_volume                     1500.01(13)
_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
_diffrn_detector                 'Bruker PHOTON area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0532
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            101710
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.498
_diffrn_reflns_theta_min         2.624
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.348
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6016
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1407 before and 0.0694 after correction.
The Ratio of minimum to maximum transmission is 0.8060.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_description       block
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.720
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5570
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0209
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0241P)^2^+1.6844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0551
_refine_ls_wR_factor_ref         0.0566
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5132
_reflns_number_total             5570
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00588d2.cif
_cod_data_source_block           bruenig140717
_cod_depositor_comments
'Adding full bibliography for 7034397--7034398.cif.'
_cod_database_code               7034397
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Others
 Fixed Sof: H6AA(0.6) H6AB(0.6) H6BC(0.4) H6BD(0.4) H3AA(0.6) H3AB(0.6)
 H3BC(0.4) H3BD(0.4) C4(0.6) H4A(0.6) H4B(0.6) C5(0.6) H5A(0.6) H5B(0.6)
 C5'(0.4) H5'A(0.4) H5'B(0.4) C4'(0.4) H4'A(0.4) H4'B(0.4)
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C1(H1A,H1B), C6(H6AA,H6AB), C6(H6BC,H6BD), C3(H3AA,H3AB),
 C3(H3BC,H3BD), C4(H4A,H4B), C5(H5A,H5B), C5'(H5'A,H5'B), C4'(H4'A,H4'B)
3.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C16(H16), C31(H31), C17(H17), C32(H32), C35(H35), C24(H24),
 C25(H25), C21(H21), C33(H33), C12(H12), C23(H23), C22(H22), C34(H34)
;
_smtbx_masks_special_details
'approx. 1/3 of a molecule of THF has 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'