Coordination versus hydrogen bonds in the structures of different tris(pyridin-2-yl)phosphoric triamide derivatives
Sebghati, Marjan; Tarahhomi, Atekeh; Bozorgvar, Marjan Sadat; Dumitrescu, Dan G.; van der Lee, Arie; RSC Advances 11 (2021) 8178–8197; doi:10.1039/D0RA10539B

data_7242300
_publ_section_title
;
 Coordination versus hydrogen bonds in the structures of different
 tris(pyridin-2-yl)phosphoric triamide derivatives
;
_journal_issue                   14
_journal_name_full               'RSC Advances'
_journal_page_first              8178
_journal_page_last               8197
_journal_paper_doi               10.1039/D0RA10539B
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         '2(C15 H16 N6 O P), 2(C15 H15 N6 O P), H2 O'
_chemical_formula_sum            'C60 H64 N24 O5 P4'
_chemical_formula_weight         1325.23
_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'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-26 deposited with the CCDC.	2021-02-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.35(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.568(2)
_cell_length_b                   13.475(3)
_cell_length_c                   21.853(4)
_cell_measurement_reflns_used    33356
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.672
_cell_measurement_theta_min      1.749
_cell_volume                     3109.3(11)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Arinax MD2S/Pilatus 6M'
_diffrn_measurement_method       'rotating crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_unetI/netI     0.0158
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            44499
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         27.672
_diffrn_reflns_theta_min         1.749
_diffrn_source                   SCW
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.969
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_description       prism
_exptl_crystal_F_000             1817
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       0.0610(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         7572
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0551P)^2^+1.1480P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.0947
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7346
_reflns_number_total             7572
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra10539b2.cif
_cod_data_source_block           ms2k_c1
_cod_database_code               7242300
_shelx_shelxl_version_number     2018/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C1-H1
 0.98 with sigma of 0.02
 C0-H0
 0.98 with sigma of 0.02
3. Others
 Fixed Sof: C0(0.5) N0(0.5) O1(0.5) H1A(0.5) H1B(0.5) N0AA(0.5) C1(0.5)
4.a Free rotating group:
 O1(H1A,H1B)
;
_olex2_submission_special_instructions 'No special instructions were received'