A stable lanthanum hydroxamate metal-organic framework with radical character and electrical conductivity
Yan, Yong; Zhang, Ningning; Fuhrmann, Daniel; Merker, Stefan Jens; Krautscheid, Harald; Dalton Transactions  (2022) –; doi:10.1039/D2DT02340G

data_7711357
_publ_section_title
;
 A stable lanthanum hydroxamate metal-organic framework with radical
 character and electrical conductivity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02340G
_journal_year                    2022
_chemical_formula_moiety
'C14 H8 La N2 O8, 2(H2 O), 1[Cl], 0.75[C4 H9 N O]'
_chemical_formula_sum            'C17 H18.75 Cl La N2.75 O10.75'
_chemical_formula_weight         607.96
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
SHELXL-2014/7
;
_audit_update_record
;
2022-09-15 deposited with the CCDC.	2022-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.908(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.2116(14)
_cell_length_b                   14.8074(11)
_cell_length_c                   8.5126(7)
_cell_measurement_reflns_used    14102
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      70.01
_cell_measurement_theta_min      3.75
_cell_volume                     2385.5(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-AREA'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9350
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         70.631
_diffrn_reflns_theta_min         3.790
_diffrn_source                   'GeniX 3D HF Cu'
_exptl_absorpt_coefficient_mu    15.397
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4624
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.024
_refine_diff_density_max         0.915
_refine_diff_density_min         -0.846
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         2257
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0335
_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^)+(0.0705P)^2^+1.9807P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0916
_refine_ls_wR_factor_ref         0.0927
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2106
_reflns_number_total             2257
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02340g2.cif
_cod_data_source_block           La-ONDI
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7711357
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.372
_shelx_estimated_absorpt_t_max   0.709
_platon_squeeze_special_details
;
A solvent mask was calculated and 246 electrons were 
found in a volume of 910\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 1[Cl] per Formula Unit 
which account for 68 electrons per unit cell.
0.75[C4H9NO] per Formula Unit account for 144 electrons per unit cell.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Riding coordinates:
 O2W(H2WA,H2WB)
2.b Rotating group:
 O1W(H1WA,H1WB)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4)
;
_shelx_res_checksum              2578
_shelx_fab_checksum              3041