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_7242301
_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         '0.5(C6 H6 Cu2 O12), C2 H8 N'
_chemical_formula_sum            'C5 H11 Cu N O6'
_chemical_formula_weight         244.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_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                 95.746(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5393(16)
_cell_length_b                   8.6391(6)
_cell_length_c                   8.8358(9)
_cell_measurement_reflns_used    1136
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.1900
_cell_measurement_theta_min      2.7160
_cell_volume                     876.41(16)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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 0.959
_diffrn_measured_fraction_theta_max 0.793
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      0.00 180.00   0.50    0.13    --    0.00   0.00   0.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dectris-CrysAlisPro-abstract goniometer imported dectris images'
_diffrn_measurement_method       'rotating crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.959
_diffrn_reflns_Laue_measured_fraction_max 0.793
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3048
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.793
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         31.758
_diffrn_reflns_theta_min         2.906
_diffrn_source                   SCW
_exptl_absorpt_coefficient_mu    2.394
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.15306
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            light_blue
_exptl_crystal_density_diffrn    1.854
_exptl_crystal_description       prism
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.371
_refine_diff_density_min         -1.028
_refine_diff_density_rms         0.246
_refine_ls_extinction_coef       0.005(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     64
_refine_ls_number_reflns         1239
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.171
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0734
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1996P)^2^+0.0925P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2243
_refine_ls_wR_factor_ref         0.2824
_reflns_Friedel_coverage         0.000
_reflns_number_gt                951
_reflns_number_total             1239
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra10539b2.cif
_cod_data_source_block           mb1k_c3__twin1
_cod_database_code               7242301
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H00A(0.5) H00B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 N005(H00A,H00B)
3.b Aromatic/amide H refined with riding coordinates:
 C006(H006), C008(H008)
3.c Idealised Me refined as rotating group:
 C007(H00C,H00D,H00E)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;