Supramolecular motifs formed by CH3/Cl-substituted arene groups: evidence for structural differences in thiophosphoramides and similarities in their complexes
Hosseinpoor, Saeed; Pourayoubi, Mehrdad; Zmeškalová, Eliška; Poupon, Morgane; RSC Advances 14 (2024) 32206–32220; doi:10.1039/D4RA05281A

data_7249454
_publ_section_title
;
 Supramolecular motifs formed by CH3/Cl-substituted arene groups: evidence
 for structural differences in thiophosphoramides and similarities in
 their complexes
;
_journal_issue                   44
_journal_name_full               'RSC Advances'
_journal_page_first              32206
_journal_page_last               32220
_journal_paper_doi               10.1039/D4RA05281A
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         'C12 H17 Cl1 N2 Ni0.50 O2 P1 S2'
_chemical_formula_sum            'C12 H17 Cl N2 Ni0.5 O2 P S2'
_chemical_formula_weight         381.19
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_update_record
;
2023-12-04 deposited with the CCDC.	2024-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                113.275(3)
_cell_angle_beta                 97.462(3)
_cell_angle_gamma                97.123(3)
_cell_formula_units_Z            2
_cell_length_a                   7.8502(2)
_cell_length_b                   10.1868(4)
_cell_length_c                   11.6914(4)
_cell_measurement_reflns_used    7760
_cell_measurement_temperature    120
_cell_measurement_theta_max      67.38
_cell_measurement_theta_min      4.18
_cell_volume                     835.66(5)
_computing_cell_refinement
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_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      120
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'focussing mirrors'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.096
_diffrn_reflns_av_unetI/netI     0.078
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12744
_diffrn_reflns_theta_full        66.285
_diffrn_reflns_theta_max         67.581
_diffrn_reflns_theta_min         4.198
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.860
_exptl_absorpt_correction_T_max  0.49
_exptl_absorpt_correction_T_min  0.15
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             394
_exptl_crystal_size_max          0.312
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.123
_refine_diff_density_max         0.76
_refine_diff_density_min         -0.81
_refine_ls_extinction_coef       18(3)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         2996
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0496
_refine_ls_shift/su_max          0.0002613
_refine_ls_shift/su_mean         0.0000195
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.09P)^2^ + 0.82P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1414
_refine_ls_wR_factor_gt          0.1338
_refine_ls_wR_factor_ref         0.1414
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              11
_reflns_limit_k_min              -12
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                2716
_reflns_number_total             2996
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.08
_oxford_diffrn_Wilson_scale      0.02
_oxford_refine_ls_r_factor_ref   0.0534
_oxford_refine_ls_scale          8.7(6)
_oxford_reflns_number_all        2996
_cod_data_source_file            d4ra05281a2.cif
_cod_data_source_block           I_CCDC1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C12 H17 Cl1 N2 Ni0.50 O2 P1 S2'
_cod_database_code               7249454
_oxford_refine_reflns_threshold_expression I>-3.0\s(I)
_oxford_refine_ls_r_factor_all   0.0534
_oxford_refine_ls_wr_factor_all  0.1414