3D isomorphous lanthanide coordination polymers displaying magnetic refrigeration, slow magnetic relaxation and tunable proton conduction.
Bera, Siba Prasad; Mondal, Arpan; Roy, Subhadip; Dey, Bijoy; Santra, Atanu; Konar, Sanjit; Dalton transactions (Cambridge, England : 2003) 47 (2018) 15405–15415; doi:10.1039/c8dt03498b

data_7047690
_publ_section_title
;
 3D isomorphous lanthanide coordination polymers displaying magnetic
 refrigeration, slow magnetic relaxation and tunable proton conduction.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15405
_journal_page_last               15415
_journal_paper_doi               10.1039/c8dt03498b
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'C28 H32 Ho4 O34 S84, 4.6(H2 O), 1.4(C2 H3 N1)'
_chemical_formula_sum            'C30.8 H45.4 Ho4 N1.4 O38.6 S4'
_chemical_formula_weight         1840.84
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-01-23
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2017.12.08 svn.r3473 for OlexSys, GUI svn.r5356)
;
_audit_update_record
;
2018-04-20 deposited with the CCDC.
2018-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.8759(6)
_cell_length_b                   12.8759(6)
_cell_length_c                   16.2369(7)
_cell_measurement_reflns_used    6681
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      33.288
_cell_measurement_theta_min      3.364
_cell_volume                     2691.9(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7832
_diffrn_reflns_point_group_measured_fraction_full 0.917
_diffrn_reflns_point_group_measured_fraction_max 0.876
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.990
_diffrn_reflns_theta_min         2.509
_exptl_absorpt_coefficient_mu    6.077
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.5159
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.0931 before and 0.0502 after correction. The Ratio of minimum to maximum transmission is 0.6911. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'pale pink'
_exptl_crystal_density_diffrn    2.271
_exptl_crystal_description       block
_exptl_crystal_F_000             1762
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details
;
 Flack x determined using 1337 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.039(6)
_refine_ls_extinction_coef       0.00024(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         3441
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0208
_refine_ls_R_factor_gt           0.0201
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0073P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0395
_refine_ls_wR_factor_ref         0.0397
_reflns_Friedel_coverage         0.700
_reflns_Friedel_fraction_full    0.828
_reflns_Friedel_fraction_max     0.748
_reflns_number_gt                3368
_reflns_number_total             3441
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03498b2.cif
_cod_data_source_block           CP_3
_cod_depositor_comments
'Adding full bibliography for 7047688--7047691.cif.'
_cod_original_cell_volume        2691.9(3)
_cod_original_formula_sum        'C30.80 H45.40 Ho4 N1.40 O38.60 S4'
_cod_database_code               7047690
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O2L-H2LA = O2L-H2LB
 0.85 with sigma of 0.02
 O1L-H1LA = O1L-H1LB
 0.85 with sigma of 0.02
 C9-C1AA
 1.456 with sigma of 0.01
 N10-C1AA
 2.593 with sigma of 0.02
 H2LA-H2LB
 1.34 with sigma of 0.04
 H1LA-H1LB
 1.34 with sigma of 0.04
 Ho1-H2LA \\sim Ho1-H2LB
 with sigma of 0.02
 Ho1-H1LA \\sim Ho1-H1LB
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1AA \\sim C9 \\sim N10: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(C1AA) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 C1AA, C9, N10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N10, C1AA, C9
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: C1AA(0.35) HB(0.35) HC(0.35) HD(0.35) C9(0.35) N10(0.35)
 O0AA(0.15) HE(0.15) HF(0.15)
6.a Riding coordinates:
 O0AA(HE,HF)
6.b Free rotating group:
 O1W(H,HA)
6.c Ternary CH refined with riding coordinates:
 O1(H1)
6.d Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C3(H3)
6.e Idealised Me refined as rotating group:
 C1AA(HB,HC,HD)
;
_shelx_res_checksum              80100
_olex2_submission_special_instructions 'No special instructions were received'