Three's company: co-crystallization of a self-assembled S4 metallacyclophane with two diastereomeric metallacycle intermediates
Lindquist, Nathan R.; Carter, Timothy G.; Cangelosi, Virginia M.; Zakharov, Lev N.; Johnson, Darren W.; Chemical Communications 46 (2010) 3505–; doi:10.1039/b927034e

data_7105569
_publ_section_title
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 Three's company: co-crystallization of a self-assembled S4
 metallacyclophane with two diastereomeric metallacycle intermediates
;
_journal_issue                   20
_journal_name_full               'Chemical Communications'
_journal_page_first              3505
_journal_paper_doi               10.1039/b927034e
_journal_volume                  46
_journal_year                    2010
_chemical_formula_sum            'C24 H24 As4 Cl12 S8'
_chemical_formula_weight         1293.99
_chemical_name_systematic
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?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXLTL
_cell_angle_alpha                90.00
_cell_angle_beta                 93.0860(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.9104(11)
_cell_length_b                   25.7564(16)
_cell_length_c                   18.9947(12)
_cell_measurement_reflns_used    7355
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.33
_cell_measurement_theta_min      2.20
_cell_volume                     8749.7(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector Bruker Apex'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            97922
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    4.166
_exptl_absorpt_correction_T_max  0.6348
_exptl_absorpt_correction_T_min  0.3491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.965
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5056
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
In the crystal structure there are four solvent molecules, C2H2Cl4.
Two of them are highly disordered and were treated by SQUEEZE
[Van der Sluis,P. & Spek, A.L. (1990) Acta Cryst., Sect.A,A46,194-201.].
Corrections of the X-ray data by SQUEEZE (645 electron/cell);
the required values (656 electron/cell) for eight solvent molecules
in the full unit cell.
;
_refine_diff_density_max         2.710
_refine_diff_density_min         -1.576
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.286
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         19054
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.286
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0717P)^2^+14.3914P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1486
_refine_ls_wR_factor_ref         0.1554
_reflns_number_gt                15435
_reflns_number_total             19054
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b927034e.txt
_cod_data_source_block           nath1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7105569