A combined X-ray crystallography and theoretical study of N—H···O<i>X</i> (<i>X</i> is =P and —C) hydrogen bonds in two new structures with a (C—O)~2~(N)P(=<i>Y</i>) (<i>Y</i> is O and S) skeleton
Vahdani Alviri, Banafsheh; Pourayoubi, Mehrdad; Farhadipour, Abolghasem; Nečas, Marek; Bertolasi, Valerio; Acta Crystallographica Section C 74 (2018) –; doi:10.1107/S2053229618014006

data_2021341
_publ_section_title
;
 A combined X-ray crystallography and theoretical study of
 N---H&#x00B7;&#x00B7;&#x00B7;O<i>X</i> (<i>X</i> is =P and ---C) hydrogen
 bonds in two new structures with a (C---O)~2~(N)P(=<i>Y</i>) (<i>Y</i> is
 O and S) skeleton
;
_journal_coeditor_code           CU3131
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229618014006
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C30 H32 N2 O6 P2'
_chemical_formula_moiety         'C30 H32 N2 O6 P2'
_chemical_formula_sum            'C30 H32 N2 O6 P2'
_chemical_formula_weight         578.51
_chemical_name_systematic
<i>N</i>,<i>N</i>'-(Cyclohexane-1,4-diyl)bis(<i>O</i>,<i>O</i>'-diphenylphosphoramide)
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                101.229(4)
_cell_angle_beta                 105.716(4)
_cell_angle_gamma                109.782(4)
_cell_formula_units_Z            2
_cell_length_a                   10.2789(5)
_cell_length_b                   10.8253(4)
_cell_length_c                   15.0200(6)
_cell_measurement_reflns_used    12958
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.8340
_cell_measurement_theta_min      3.1630
_cell_volume                     1436.22(13)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
<i>CrystalClear-SM Expert</i> (Rigaku, 2014)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'AFC11 (Right): Eulerian 3 circle CCD'
_diffrn_measurement_method       'Profile data from \w-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15732
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.346
_diffrn_reflns_theta_min         3.006
_diffrn_source                   'Rotating Anode MicroMax-007HF DW 1.2 kW'
_exptl_absorpt_coefficient_mu    0.198
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89340
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_description       block
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.299
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 3782 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.09(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         9396
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0467P)^2^+0.2585P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0775
_reflns_number_gt                9009
_reflns_number_total             9396
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cu3131sup1.cif
_cod_data_source_block           bv91
_cod_original_cell_volume        1436.22(12)
_cod_database_code               2021341
_cod_database_fobs_code          2021341
_shelx_estimated_absorpt_t_min   0.962
_shelx_estimated_absorpt_t_max   0.981
_shelx_hkl_checksum              80616
_shelx_res_checksum              34415