One-Pot Three-Component Condensation Synthesis and Structural Features of Organophosphorus-Sulfur Macrocycles.
Hua, Guoxiong; Du, Junyi; Cordes, David B.; Slawin, Alexandra M. Z.; Woollins, J. Derek; The Journal of organic chemistry 81 (2016) 4210–4225; doi:10.1021/acs.joc.6b00573

data_4036809
_publ_section_title
;
 One-Pot Three-Component Condensation Synthesis and Structural Features of
 Organophosphorus-Sulfur Macrocycles.
;
_journal_issue                   10
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              4210
_journal_page_last               4225
_journal_paper_doi               10.1021/acs.joc.6b00573
_journal_volume                  81
_journal_year                    2016
_chemical_formula_moiety         'C32 H34 Fe2 P2 S6'
_chemical_formula_sum            'C32 H34 Fe2 P2 S6'
_chemical_formula_weight         784.62
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_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.297(8)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   23.798(3)
_cell_length_b                   7.4405(9)
_cell_length_c                   37.885(3)
_cell_measurement_reflns_used    5644
_cell_measurement_temperature    173
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      1.71
_cell_volume                     6708.2(13)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b28'
_computing_data_collection
'CrystalClear-SM Expert 2.1 b28 (Rigaku, 2013)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b28'
_computing_molecular_graphics    'CrystalStructure 4.1'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1898
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            43287
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.411
_diffrn_reflns_theta_min         1.075
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.356
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.568
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             3232.00
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.10
_refine_diff_density_min         -0.34
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6151
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0697
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0818P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1735
_reflns_number_gt                3922
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_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            18.cif
_cod_data_source_block           HW345
_cod_original_cell_volume        6708.1(13)
_cod_database_code               4036809