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_7242303
_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         'C30 H32 Co N12 O2 P2, 3.053(Cl)'
_chemical_formula_sum            'C30 H32 Cl3.05 Co N12 O2 P2'
_chemical_formula_weight         821.77
_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   geom
_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                 93.06(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5130(17)
_cell_length_b                   15.816(3)
_cell_length_c                   26.981(5)
_cell_measurement_reflns_used    58514
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.666
_cell_measurement_theta_min      1.470
_cell_volume                     3627.6(12)
_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 0.988
_diffrn_measured_fraction_theta_max 0.982
_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  0.0228
_diffrn_reflns_av_unetI/netI     0.0143
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            51573
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         27.666
_diffrn_reflns_theta_min         1.470
_diffrn_source                   SCW
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.793
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_description       prism
_exptl_crystal_F_000             1683.6
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.936
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       0.0096(6)
_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   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         8709
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0821P)^2^+3.1761P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1503
_refine_ls_wR_factor_ref         0.1598
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7105
_reflns_number_total             8709
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra10539b2.cif
_cod_data_source_block           ms3k_c2
_cod_original_cell_volume        3627.6(13)
_cod_database_code               7242303
_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
2. Others
 1*[Sof(Cl01)]+1*[Sof(Cl3)]+1*[Sof(Cl1)]+1*[Sof(Cl06)]+1*[Sof(Cl0A)]+1*
 [Sof(Cl2)]+1*[Sof(Cl4)]+1*[Sof(Cl1A)]+1*[Sof(Cl05)]+1*[Sof(Cl2A)]=3 with esd
 of 0.01
 1*[Sof(Cl01)]+1*[Sof(Cl3)]+1*[Sof(Cl1)]+1*[Sof(Cl06)]+1*[Sof(Cl0A)]+1*
 [Sof(Cl2)]+1*[Sof(Cl4)]+1*[Sof(Cl1A)]+1*[Sof(Cl05)]+1*[Sof(Cl2A)]=3 with esd
 of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 N00D(H00D), N00E(H00E), N00F(H00F), N00G(H00G), N00H(H00H), N00I(H00I),
 N00J(H00J), N00K(H00K), C00L(H00L), C00N(H00N), C00Q(H00Q), C00S(H00S),
 C00T(H00T), C00U(H00U), C00V(H00V), C00W(H00W), C00X(H00X), C00Y(H00Y),
 C00Z(H00Z), C010(H010), C012(H012), C013(H013), C014(H014), C015(H015),
 C016(H016), C017(H017), C01A(H01A), C01D(H01D), C01E(H01E), C01F(H01F),
 C01G(H01G), C01H(H01H)
;
_olex2_submission_special_instructions 'No special instructions were received'