Sensing and extraction of hazardous metals by di-phosphonates of heterocycles: a combined experimental and theoretical study
Konopkina, Ekaterina; Pozdeev, Anton; Kalle, Paulina; Kirsanov, Dmitry; Smol'yanov, Nikolai; Kirsanova, Anna A.; Kalmykov, Stepan; Petrov, Vladimir G.; Borisova, Nataliya E.; Matveev, Petr I.; Dalton Transactions  (2023) –; doi:10.1039/D3DT01534C

data_7713690
_publ_section_title
;
 Sensing and extraction of hazardous metals by di-phosphonates of
 heterocycles: a combined experimental and theoretical study
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01534C
_journal_year                    2023
_chemical_formula_moiety         'C34 H62 Cd2 Cl3.6 N2.4 O13.2 P4'
_chemical_formula_sum            'C34 H62 Cd2 Cl3.6 N2.4 O13.2 P4'
_chemical_formula_weight         1191.96
_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             2023-06-27
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-07-04 deposited with the CCDC.	2023-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.798(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.8333(9)
_cell_length_b                   16.1328(11)
_cell_length_c                   13.2377(9)
_cell_measurement_reflns_used    9958
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.759
_cell_measurement_theta_min      2.280
_cell_volume                     2562.1(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'APEX3 v.2017.3_0 (Bruker AXS, 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker SMART APEX-II'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            43896
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.785
_diffrn_reflns_theta_min         2.280
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_target            Mo
_diffrn_source_type              'fine-focus sealed X-ray tube'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.198
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6138
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1017 before and 0.0559 after correction.
The Ratio of minimum to maximum transmission is 0.8232.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_description       plate
_exptl_crystal_F_000             1211
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.052
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         5817
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0199P)^2^+5.0836P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0801
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5333
_reflns_number_total             5817
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01534c2.cif
_cod_data_source_block           cdrik10
_cod_original_formula_sum        'C34 H62 Cd2 Cl3.60 N2.40 O13.20 P4'
_cod_database_code               7713690
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.890
_shelx_estimated_absorpt_t_min   0.679
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cd1-O8
 2.4 with sigma of 0.01
 N1A-O8
 1.3 with sigma of 0.02
 O9-N1A \\sim O7-N1A
 with sigma of 0.02
3. Restrained planarity
 O7, N1A, O8, O9
 with sigma of 0.1
4. Others
 Fixed Sof: Cl1(0.8) O8(0.2) O9(0.2) O7(0.2) N1A(0.2)
5.a Ternary CH refined with riding coordinates:
 C9(H9), C6(H6), C15(H15), C12(H12)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C3(H3)
5.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C11(H11A,H11B,H11C), C8(H8A,H8B,
 H8C), C7(H7A,H7B,H7C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C14(H14A,H14B,
 H14C)
;
_shelx_res_checksum              39066
_olex2_date_sample_completion    2022-10-18
_olex2_date_sample_data_collection 2022-10-18
_olex2_date_sample_submission    2022-10-18
_olex2_submission_special_instructions 'No special instructions were received'