Synthesis and structures of [S[double bond, length as m-dash](H)P(μ-NR)]2, potential building blocks for inorganic phosphorus-sulfur macrocycles.
Benson, Callum G. M.; Vasilenko, Vladislav; García-Rodríguez, Raúl; Bond, Andrew D.; González Calera, Silvia; Gade, Lutz H.; Wright, Dominic S.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 14242–14247; doi:10.1039/c5dt02069g

data_7035699
_publ_section_title
;
 Synthesis and structures of [S[double bond, length as
 m-dash](H)P(\m-NR)]2, potential building blocks for inorganic
 phosphorus-sulfur macrocycles.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14242
_journal_page_last               14247
_journal_paper_doi               10.1039/c5dt02069g
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C24 H36 N2 P2 S2'
_chemical_formula_sum            'C24 H36 N2 P2 S2'
_chemical_formula_weight         478.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-04-30 deposited with the CCDC.
2015-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.646(7)
_cell_angle_gamma                90
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_cell_length_b                   10.1458(17)
_cell_length_c                   15.541(3)
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_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      18.38
_cell_measurement_theta_min      2.41
_cell_volume                     1292.5(4)
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
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_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL
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_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART X2S'
_diffrn_measurement_method       \f-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0895
_diffrn_reflns_av_unetI/netI     0.0591
_diffrn_reflns_Laue_measured_fraction_full 0.997
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_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
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_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11418
_diffrn_reflns_point_group_measured_fraction_full 0.997
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_diffrn_reflns_theta_full        22.776
_diffrn_reflns_theta_max         22.776
_diffrn_reflns_theta_min         2.413
_diffrn_source                   sealed-tube
_exptl_absorpt_coefficient_mu    0.344
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_exptl_absorpt_correction_T_min  0.8237
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_description       block
_exptl_crystal_F_000             512
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Pentane'
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_exptl_crystal_size_min          0.100
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_refine_diff_density_min         -0.229
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         1743
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0279P)^2^+0.4487P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0763
_refine_ls_wR_factor_ref         0.0869
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1231
_reflns_number_total             1743
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02069g2.cif
_cod_data_source_block           IIIB
_cod_depositor_comments
'Adding full bibliography for 7035698--7035700.cif.'
_cod_database_code               7035699
_shelx_estimated_absorpt_t_min   0.847
_shelx_estimated_absorpt_t_max   0.966
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