Carbonate and phosphite encaged in the frameworks constructed by square lanthanum aminopolycarboxylates and sodium chlorides
Wang, Si-Yuan; Gao, Song; Dai, Jun-Wei; Shi, Yan-Ru; Dong, Xin; Weng, Weizheng; Zhou, Zhao-Hui; Dalton Transactions  (2019) –; doi:10.1039/C8DT04940H

data_7048819
_publ_section_title
;
 Carbonate and phosphite encaged in the frameworks constructed by square
 lanthanum aminopolycarboxylates and sodium chlorides
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C8DT04940H
_journal_year                    2019
_chemical_formula_moiety         '0.5(C88 H112 Cl16 La8 N16 Na40 O96)'
_chemical_formula_sum            'C44 H56 Cl8 La4 N8 Na20 O48'
_chemical_formula_weight         2764.00
_space_group_crystal_system      tetragonal
_space_group_IT_number           125
_space_group_name_Hall           '-P 4a 2b'
_space_group_name_H-M_alt        'P 4/n b m'
_symmetry_space_group_name_Hall  '-P 4a 2b'
_symmetry_space_group_name_H-M   'P 4/n b m :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-04-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2018-12-11 deposited with the CCDC.
2019-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.0220(3)
_cell_length_b                   21.0220(3)
_cell_length_c                   9.5449(3)
_cell_measurement_reflns_used    3385
_cell_measurement_temperature    173
_cell_measurement_theta_max      29.1590
_cell_measurement_theta_min      3.0410
_cell_volume                     4218.13(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1903
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.913
_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    -46.00   1.00   1.00   25.00    --  -22.85  57.00 150.00   47
  2  \w    -86.00   0.00   1.00   25.00    --  -22.85 -57.00 -90.00   86
  3  \w    -48.00 -23.00   1.00   25.00    --  -22.85  77.00 -60.00   25
  4  \w    -34.00  -8.00   1.00   25.00    --  -22.85  19.00 -30.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0163172000
_diffrn_orient_matrix_UB_12      -0.0279231000
_diffrn_orient_matrix_UB_13      -0.0207686000
_diffrn_orient_matrix_UB_21      0.0294181000
_diffrn_orient_matrix_UB_22      0.0144158000
_diffrn_orient_matrix_UB_23      0.0180392000
_diffrn_orient_matrix_UB_31      -0.0027338000
_diffrn_orient_matrix_UB_32      -0.0122338000
_diffrn_orient_matrix_UB_33      0.0690535000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.913
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            14428
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.913
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.837
_diffrn_reflns_theta_min         2.883
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.447
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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    2.176
_exptl_crystal_description       block
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.991
_refine_diff_density_min         -1.825
_refine_diff_density_rms         0.224
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.208
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         2886
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.206
_refine_ls_R_factor_all          0.0917
_refine_ls_R_factor_gt           0.0805
_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^)+(0.0223P)^2^+133.1091P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1609
_refine_ls_wR_factor_ref         0.1657
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2462
_reflns_number_total             2886
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04940h2.cif
_cod_data_source_block           exp_16295
_cod_original_cell_volume        4218.13(18)
_cod_database_code               7048819
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.72
_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,H) groups
2. Rigid bond restraints
 C6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Others
 Fixed Sof: Cl2(0.33333) Cl1(0.16667) H1WA(0.5) H1WB(0.5)
5.a Rotating group:
 O1W(H1WA,H1WB)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B)
;
_shelx_res_checksum              10387
_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 1.039
_oxdiff_exptl_absorpt_empirical_full_min 0.952