Metal phosphonates as heterogeneous catalysts for highly efficient chemical fixation of CO2 under mild conditions
Wang, Yi-xin; Zhou, Jing-hui; Xiong, Jun; Huang, Wan-qi; Li, Quan; Min, Xue; Li, Ming; CrystEngComm  (2022) –; doi:10.1039/D2CE01162J

data_7245728
_publ_section_title
;
 Metal phosphonates as heterogeneous catalysts for highly efficient
 chemical fixation of CO2 under mild conditions
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE01162J
_journal_year                    2022
_chemical_formula_moiety         'C5 H11 Cd1.5 N2 O9 P2, H2 O'
_chemical_formula_sum            'C5 H13 Cd1.5 N2 O10 P2'
_chemical_formula_weight         491.71
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_audit_creation_date             2022-05-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-06-06 deposited with the CCDC.	2022-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                89.108(6)
_cell_angle_beta                 85.440(6)
_cell_angle_gamma                75.799(6)
_cell_formula_units_Z            2
_cell_length_a                   5.1177(3)
_cell_length_b                   9.8637(7)
_cell_length_c                   12.9604(9)
_cell_measurement_reflns_used    2672
_cell_measurement_temperature    273
_cell_measurement_theta_max      29.0110
_cell_measurement_theta_min      4.1170
_cell_volume                     632.23(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      273.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0353
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.872
_diffrn_measured_fraction_theta_max 0.872
_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    -35.00  53.00   1.00    7.19    --  -15.92  37.00 -90.00   88
  2  \w    -10.00  42.00   1.00    7.19    --   16.85  77.00  90.00   52
  3  \w    -10.00  42.00   1.00    7.19    --   16.85  77.00-180.00   52
  4  \w    -10.00  42.00   1.00    7.19    --   16.85  77.00   0.00   52
  5  \w    -50.00   7.00   1.00    7.19    --   16.85 -57.00  60.00   57
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0654953000
_diffrn_orient_matrix_UB_12      0.0374596000
_diffrn_orient_matrix_UB_13      0.0449461000
_diffrn_orient_matrix_UB_21      0.0340002000
_diffrn_orient_matrix_UB_22      -0.0620108000
_diffrn_orient_matrix_UB_23      0.0296471000
_diffrn_orient_matrix_UB_31      0.1229481000
_diffrn_orient_matrix_UB_32      0.0159296000
_diffrn_orient_matrix_UB_33      0.0107435000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.872
_diffrn_reflns_Laue_measured_fraction_max 0.872
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3625
_diffrn_reflns_point_group_measured_fraction_full 0.872
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.799
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.853
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82320
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.121a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.583
_exptl_crystal_description       block
_exptl_crystal_F_000             478
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         1939
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0358P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0688
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1781
_reflns_number_total             1939
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01162j2.cif
_cod_data_source_block           mx-1_auto
_cod_original_cell_volume        632.23(8)
_cod_original_formula_sum        'C5 H13 Cd1.50 N2 O10 P2'
_cod_database_code               7245728
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.599
_shelx_estimated_absorpt_t_min   0.481
_reflns_odcompleteness_completeness 86.14
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O10(H10A,H10B)
2.b Rotating group:
 O9(H9A,H9B), O8(H8A,H8B)
2.c Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B)
2.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C2(H2A)
2.e Idealised tetrahedral OH refined as rotating group:
 O2(H2), O1(H1A)
;
_shelx_res_checksum              85216
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.272
_oxdiff_exptl_absorpt_empirical_full_min 0.837