Analysis of N—H···O hydrogen bonds in new C(O)—NH—P(O)-based phosphoric triamides and analogous structures deposited in the Cambridge Structural Database
Pourayoubi, Mehrdad; Toghraee, Maryam; Divjakovic, Vladimir; van der Lee, Arie; Mancilla Percino, Teresa; Leyva Ramírez, Marco A.; Saneei, Anahid; Acta Crystallographica Section B 69 (2013) 184–194; doi:10.1107/S2052519213002650

data_2105940
_publ_section_title
;
 Analysis of N---H&#x00B7;&#x00B7;&#x00B7;O hydrogen bonds in new
 C(O)---NH---P(O)-based phosphoric triamides and analogous structures
 deposited in the Cambridge Structural Database
;
_journal_coeditor_code           DK5007
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              184
_journal_page_last               194
_journal_paper_doi               10.1107/S2052519213002650
_journal_volume                  69
_journal_year                    2013
_chemical_formula_moiety         'C15 H24 Cl2 N3 O2 P'
_chemical_formula_sum            'C15 H24 Cl2 N3 O2 P'
_chemical_formula_weight         380.24
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_cell_angle_alpha                66.278(3)
_cell_angle_beta                 67.729(2)
_cell_angle_gamma                84.121(2)
_cell_formula_units_Z            2
_cell_length_a                   9.7455(2)
_cell_length_b                   10.0122(3)
_cell_length_c                   11.7163(3)
_cell_measurement_reflns_used    11215
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.9997
_cell_measurement_theta_min      2.0403
_cell_volume                     966.85(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 16.0143
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.058
_diffrn_reflns_av_sigmaI/netI    0.091
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            43311
_diffrn_reflns_theta_full        25.285
_diffrn_reflns_theta_max         29.064
_diffrn_reflns_theta_min         2.044
_exptl_absorpt_coefficient_mu    0.430
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93320
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'long block'
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.55
_refine_diff_density_min         -0.52
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9719
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         4853
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.0002645
_refine_ls_shift/su_mean         0.0000259
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
 Method = Robust Weighting (Prince, 1982)
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
 A~i~ are:
 0.119E+04 0.124E+04 666. 226. -17.0
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0674
_refine_ls_wR_factor_gt          0.0609
_refine_ls_wR_factor_ref         0.0674
_reflns_number_gt                3805
_reflns_number_total             4853
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            dk5007sup1.cif
_cod_data_source_block           III
_cod_original_cell_volume        966.84(5)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               2105940
_cod_database_fobs_code          2105940