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_7048820
_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         '0.25(C240 H288 K48 La16 N32 O252), 4(O)'
_chemical_formula_sum            'C60 H118 K12 La4 N8 O67'
_chemical_formula_weight         3048.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-06-05
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-12-11 deposited with the CCDC.
2019-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.532(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.8933(10)
_cell_length_b                   9.4679(4)
_cell_length_c                   34.2291(14)
_cell_measurement_temperature    173.15
_cell_volume                     10406.0(7)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_av_unetI/netI     0.0722
_diffrn_reflns_Laue_measured_fraction_full 0.951
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            23750
_diffrn_reflns_point_group_measured_fraction_full 0.951
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.115
_exptl_absorpt_coefficient_mu    2.202
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92938
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.946
_exptl_crystal_description       block
_exptl_crystal_F_000             6104
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.602
_refine_diff_density_min         -1.351
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     681
_refine_ls_number_reflns         8712
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0748
_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^)+(0.0331P)^2^+256.5792P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1435
_refine_ls_wR_factor_ref         0.1529
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6855
_reflns_number_total             8712
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04940h2.cif
_cod_data_source_block           r
_cod_database_code               7048820
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.898
_shelx_estimated_absorpt_t_min   0.473
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O22) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.01
3.a Ternary CH refined with riding coordinates:
 C19(H19), C20(H20), C29(H29), C30(H30)
3.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C13(H13A,H13B), C15(H15A,H15B), C17(H17A,H17B), C21(H21A,
 H21B), C23(H23A,H23B), C25(H25A,H25B), C27(H27A,H27B), C31(H31A,H31B),
 C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B),
  C37(H37A,H37B), C38(H38A,H38B)
;
_shelx_res_checksum              9907
_olex2_submission_special_instructions 'No special instructions were received'