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_7242304
_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         'C15 H15 N6 O P, C3 H7 N O, 0.5(H2 O)'
_chemical_formula_sum            'C18 H23 N7 O2.5 P'
_chemical_formula_weight         408.40
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-24
_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                 98.25(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.625(2)
_cell_length_b                   18.707(4)
_cell_length_c                   20.479(4)
_cell_measurement_reflns_used    52157
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.667
_cell_measurement_theta_min      1.459
_cell_volume                     4028.3(14)
_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 0.997
_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  0.0318
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.997
_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       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            57512
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         27.667
_diffrn_reflns_theta_min         1.459
_diffrn_source                   SCW
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.160
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_description       prism
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       0.0765(17)
_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   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         9811
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+2.0043P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1065
_refine_ls_wR_factor_ref         0.1069
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9586
_reflns_number_total             9811
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra10539b2.cif
_cod_data_source_block           ms1k_c3
_cod_depositor_comments
;

2024-06-28
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C15 H15 N6 O P), 2(C3 H7 N O), H2 O'
_cod_original_formula_sum        'C36 H46 N14 O5 P2'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     816.81
_cod_database_code               7242304
_shelx_shelxl_version_number     2018/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Riding coordinates:
 N007(H007), N00A(H00A)
2.b Free rotating group:
 O006(H00B,H00D)
2.c Aromatic/amide H refined with riding coordinates:
 N008(H008), N009(H009), N00C(H00C), N00G(H00G), C00S(H00S), C00T(H00T),
 C00U(H00U), C00V(H00V), C00W(H00W), C00X(H00X), C00Y(H00Y), C00Z(H00Z),
 C010(H010), C011(H011), C012(H012), C013(H013), C014(H014), C015(H015),
 C016(H016), C017(H017), C018(H018), C019(H019), C01A(H01A), C01B(H01B),
 C01C(H01C), C01D(H01D), C01E(H01E), C01F(H01F), C01G(H01N), C01H(H01H)
2.d Idealised Me refined as rotating group:
 C01I(H01O,H01P,H01Q), C01J(H01R,H01S,H01T), C01K(H01G,H01I,H01J), C01L(H01K,
 H01L,H01M)
;
_olex2_submission_special_instructions 'No special instructions were received'