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_7061207
_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 H28 La2 N4 Na8 O37.5, 5[H2O]'
_chemical_formula_sum            'C23 H38 La2 N4 Na8 O42.5'
_chemical_formula_weight         1512.31
_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             2021-10-11
_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                73.795(6)
_cell_angle_beta                 85.301(5)
_cell_angle_gamma                82.669(5)
_cell_formula_units_Z            2
_cell_length_a                   12.4288(8)
_cell_length_b                   14.3340(10)
_cell_length_c                   16.0464(11)
_cell_measurement_reflns_used    3556
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.9230
_cell_measurement_theta_min      3.4570
_cell_volume                     2719.5(3)
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.1903
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.854
_diffrn_measurement_details
;
  1 omega  -45.00   52.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.6309   77.0000  120.0000 97

  2 omega  -58.00    1.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.6309  -57.0000  -60.0000 59

  3 omega  -50.00    3.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.6309  -38.0000  120.0000 53

  4 omega   -3.00   43.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.6309   57.0000  -90.0000 46

  5 omega  -91.00  -24.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.6309  -57.0000   30.0000 67

  6 omega   78.00  104.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8809 -178.0000 -180.0000 26

  7 omega  -22.00    8.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8809   97.0000  -54.0000 30

  8 omega    3.00   85.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8809   77.0000 -150.0000 82

  9 omega   70.00   95.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8809 -178.0000   60.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0214446000
_diffrn_orient_matrix_UB_12      -0.0457005000
_diffrn_orient_matrix_UB_13      0.0137736000
_diffrn_orient_matrix_UB_21      -0.0224220000
_diffrn_orient_matrix_UB_22      0.0090869000
_diffrn_orient_matrix_UB_23      -0.0411300000
_diffrn_orient_matrix_UB_31      0.0485386000
_diffrn_orient_matrix_UB_32      -0.0227270000
_diffrn_orient_matrix_UB_33      -0.0155743000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_av_unetI/netI     0.1024
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.854
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24018
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.854
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.021
_diffrn_reflns_theta_min         2.911
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.726
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95054
_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_density_diffrn    1.847
_exptl_crystal_description       block
_exptl_crystal_F_000             1492
_refine_diff_density_max         1.310
_refine_diff_density_min         -1.525
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     702
_refine_ls_number_reflns         12373
_refine_ls_number_restraints     510
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0531
_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^)+(0.0383P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1217
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9294
_reflns_number_total             12373
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05608e2.cif
_cod_data_source_block           exp_5038
_cod_depositor_comments
'Adding full bibliography for 7061206--7061210.cif.'
_cod_original_formula_sum        'C23 H38 La2 N4 Na8 O42.50'
_cod_database_code               7061207
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
O4 \\sim O16 \\sim O1 \\sim O5 \\sim O12 \\sim O24 \\sim O3 \\sim O10 \\sim O2
\\sim O8 \\sim O20 \\sim O18 \\sim O14 \\sim O25 \\sim O6 \\sim O22 \\sim O13
\\sim O17 \\sim O9 \\sim O15 \\sim O11 \\sim O7 \\sim O23 \\sim O21 \\sim O19
\\sim O7W \\sim O3W \\sim O8W \\sim O5W \\sim O2W \\sim O11W \\sim O6W \\sim
O4W \\sim O12W \\sim O1W \\sim O13W \\sim O14W \\sim O15W \\sim O9W \\sim O10W:
within 3.8A with sigma of 0.005 and sigma for terminal atoms of 0.01 within 3.8A
3. Others
 Fixed Sof: O6W(0.5) O4W(0.5) Na9(0.5) O13W(0.5) O14W(0.5) O15W(0.5)
4.a Rotating group:
 O7W(H7WA,H7WB), O11W(H11C,H11D)
4.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C8(H8A,H8B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B),
 C14(H14A,H14B), C15(H15A,H15B), C19(H19A,H19B), C20(H20A,H20B), 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              75839
_shelx_fab_checksum              78981
_olex2_submission_special_instructions 'No special instructions were received'