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_4036804
_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_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C25 H28 O2 P2 S6'
_chemical_formula_sum            'C25 H28 O2 P2 S6'
_chemical_formula_weight         614.80
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
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_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   34.2(2)
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_cell_length_c                   6.90(5)
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_cell_measurement_theta_max      25.40
_cell_measurement_theta_min      1.80
_cell_volume                     2799(3)
_computing_cell_refinement       'CrystalClear-SM Expert 3.1 b27'
_computing_data_collection
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)'
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_computing_molecular_graphics    'CrystalStructure 4.1'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0782
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_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            8618
_diffrn_reflns_point_group_measured_fraction_full 0.000
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_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.817
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.626
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.590
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1280.00
_exptl_crystal_size_max          0.120
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_refine_diff_density_max         0.23
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_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  833 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.13(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.935
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     160
_refine_ls_number_reflns         2205
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_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0198P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0580
_refine_ls_wR_factor_ref         0.0648
_reflns_number_gt                1602
_reflns_number_total             2205
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            5.cif
_cod_data_source_block           HW317-1-1-A2
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file
'/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/lists/replacement-tags.lst'.

Automatic conversion script
Id: cif_correct_tags 6909 2019-04-08 15:41:33Z antanas 
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_cod_original_cell_volume        2799(32)
_cod_database_code               4036804