Highly water-soluble dimeric and trimeric lanthanide carbonates with ethylenediaminetetraacetates as precursors of catalysts for the oxidative coupling reaction of methane
Lin, Rong-Yan; Shi, Yan-Ru; Hou, Yu-Hui; Xia, Wen-Sheng; Weng, Wei-Zheng; Zhou, Zhao-Hui; New Journal of Chemistry 46 (2022) 3707–3715; doi:10.1039/D1NJ05608E

data_7061208
_publ_section_title
;
 Highly water-soluble dimeric and trimeric lanthanide carbonates with
 ethylenediaminetetraacetates as precursors of catalysts for the oxidative
 coupling reaction of methane
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3707
_journal_page_last               3715
_journal_paper_doi               10.1039/D1NJ05608E
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C23 H30.5 Ce2 N4 Na8 O37, 5[H2O], 0.5[H2O]'
_chemical_formula_sum            'C23 H41.5 Ce2 N4 Na8 O42.5'
_chemical_formula_weight         1518.26
_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     dual
_audit_creation_date             2021-10-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2021-10-13 deposited with the CCDC.	2022-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                73.825(14)
_cell_angle_beta                 85.236(14)
_cell_angle_gamma                82.697(13)
_cell_formula_units_Z            2
_cell_length_a                   12.416(2)
_cell_length_b                   14.310(2)
_cell_length_c                   16.017(3)
_cell_measurement_reflns_used    1401
_cell_measurement_temperature    172.95(10)
_cell_measurement_theta_max      25.5210
_cell_measurement_theta_min      3.2380
_cell_volume                     2707.6(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      172.95(10)
_diffrn_detector_area_resol_mean 16.1903
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.861
_diffrn_measurement_details
;
  1 omega  -50.00   51.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.8497   38.0000  120.0000 101

  2 omega  -46.00   51.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.8497   38.0000 -150.0000 97

  3 omega  -55.00   40.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.8497   77.0000  -30.0000 95

  4 omega   57.00   82.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       24.0997  178.0000  -90.0000 25

  5 omega   31.00   74.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       24.0997   57.0000  -90.0000 43

  6 omega   67.00  104.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       24.0997  178.0000  150.0000 37

  7 omega   30.00   73.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       24.0997 -109.0000  114.0000 43

  8 omega   28.00   68.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       24.0997  -99.0000 -150.0000 40
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0232747000
_diffrn_orient_matrix_UB_12      0.0064234000
_diffrn_orient_matrix_UB_13      -0.0429260000
_diffrn_orient_matrix_UB_21      0.0314064000
_diffrn_orient_matrix_UB_22      -0.0461141000
_diffrn_orient_matrix_UB_23      0.0133546000
_diffrn_orient_matrix_UB_31      -0.0424000000
_diffrn_orient_matrix_UB_32      -0.0229625000
_diffrn_orient_matrix_UB_33      -0.0105262000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1065
_diffrn_reflns_av_unetI/netI     0.2053
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.861
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25042
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.861
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.954
_diffrn_reflns_theta_min         2.916
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.838
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97222
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.862
_exptl_crystal_description       block
_exptl_crystal_F_000             1503
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.496
_refine_diff_density_min         -1.982
_refine_diff_density_rms         0.208
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         13550
_refine_ls_number_restraints     562
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.1416
_refine_ls_R_factor_gt           0.0800
_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^)+(0.0110P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1192
_refine_ls_wR_factor_ref         0.1477
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7563
_reflns_number_total             13550
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05608e2.cif
_cod_data_source_block           exp_5314
_cod_depositor_comments
'Adding full bibliography for 7061206--7061210.cif.'
_cod_original_cell_volume        2707.5(8)
_cod_original_formula_sum        'C23 H41.50 Ce2 N4 Na8 O42.50'
_cod_database_code               7061208
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.838
_shelx_estimated_absorpt_t_min   0.710
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 H12W-O12W_$1
 1.5 with sigma of 0.02
 H9W-O9W
 0.85 with sigma of 0.02
 H11W-O11W
 0.85 with sigma of 0.02
 H11W-O23_$1
 1.9 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1 \\sim O12 \\sim O5 \\sim O2 \\sim O3 \\sim O16 \\sim O10 \\sim O24 \\sim O4
\\sim O14 \\sim O8 \\sim O20 \\sim O18 \\sim O13 \\sim O25 \\sim O22 \\sim O6
\\sim O17 \\sim O9 \\sim O7 \\sim O15 \\sim O11 \\sim O23 \\sim O19 \\sim O21
\\sim O3W \\sim O8W \\sim O10W \\sim O9W \\sim O2W \\sim O1W \\sim O5W \\sim
O11W \\sim O6W \\sim O7W \\sim O12W \\sim O13W \\sim O14W \\sim O4W: within
3.8A with sigma of 0.007 and sigma for terminal atoms of 0.014 within 3.8A
Uanis(C19) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O7W) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.016
Uanis(C19) = Uanis(C14)
4. Others
 Fixed Sof: Na9(0.5) O6W(0.5) O12W(0.5) H12W(0.5) O13W(0.5) O14W(0.5)
5.a Rotating group:
 O10W(H10A,H10B), O5W(H5WA,H5WB)
5.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C9(H9A,H9B), C12(H12A,H12B), C13(H13A,
 H13B), C16(H16A,H16B), C17(H17A,H17B), C19(H19A,H19B), C21(H21A,H21B),
 C22(H22A,H22B), C23(H23A,H23B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              82165
_shelx_fab_checksum              12879
_olex2_submission_special_instructions 'No special instructions were received'