Synthesis, structure, magnetic and magnetocaloric properties of a series of {CrIII4LnIII} complexes
Blacque, Olivier; Amjad, Asma; Caneschi, Andrea; Sorace, Lorenzo; Car, Pierre-Emmanuel; New J. Chem. 40 (2016) 3571–; doi:10.1039/C6NJ00136J

data_7055383
_publ_section_title
;
 Synthesis, structure, magnetic and magnetocaloric properties of a series
 of {CrIII4LnIII} complexes
;
_journal_issue                   4
_journal_name_full               'New J. Chem.'
_journal_page_first              3571
_journal_paper_doi               10.1039/C6NJ00136J
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'C70 H51 Cr4 N12 O18 Tb, 2(N O3), 20(H2 O)'
_chemical_formula_sum            'C70 H91 Cr4 N14 O44 Tb'
_chemical_formula_weight         2199.48
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-05-22
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_audit_update_record
;
2015-12-04 deposited with the CCDC.
2016-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.6450(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7168(3)
_cell_length_b                   24.1981(3)
_cell_length_c                   22.1270(4)
_cell_measurement_reflns_used    17498
_cell_measurement_temperature    183(1)
_cell_measurement_theta_max      75.9
_cell_measurement_theta_min      1.8
_cell_volume                     8907.3(3)
_computing_cell_refinement
;
CrysAlisPro, version 1.171.37.31d (Agilent Technologies, 2012)
;
_computing_data_collection
;
CrysAlisPro, version 1.171.37.31d (Agilent Technologies, 2012)
;
_computing_data_reduction
;
CrysAlisPro, version 1.171.36.20 (Agilent Technologies, 2012)
;
_computing_molecular_graphics
;
<i>Mercury</i> (Macrae et al., 2006)
;
_computing_publication_material
; 
Olex2 (Dolomanov et al., 2009), <i>PLATON for Windows</i> (Spek, 2003) and
<i>publCIF</i> (Westrip, 2010)
;
_computing_structure_refinement  ' SHELXL2013 (Sheldrick, 2008)'
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      183(1)
_diffrn_detector_area_resol_mean 10.3801
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0187739000
_diffrn_orient_matrix_UB_12      -0.0126874000
_diffrn_orient_matrix_UB_13      0.0681175000
_diffrn_orient_matrix_UB_21      -0.0201201000
_diffrn_orient_matrix_UB_22      -0.0613832000
_diffrn_orient_matrix_UB_23      -0.0121762000
_diffrn_orient_matrix_UB_31      0.0884540000
_diffrn_orient_matrix_UB_32      -0.0112634000
_diffrn_orient_matrix_UB_33      -0.0100190000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0576
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            66132
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.248
_diffrn_reflns_theta_min         2.713
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.624
_exptl_absorpt_correction_T_max  0.799
_exptl_absorpt_correction_T_min  0.424
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_description       needle
_exptl_crystal_F_000             4488
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.406
_refine_diff_density_min         -0.958
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1096
_refine_ls_number_reflns         16303
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0705
_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^)+(0.1187P)^2^+37.8602P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2068
_refine_ls_wR_factor_ref         0.2262
_reflns_number_gt                12153
_reflns_number_total             16303
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj00136j2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7055381--7055384.cif.'
_cod_database_code               7055383
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O22A-O23A = O23A-O24A = O24A-O22A = O22B-O23B = O23B-O24B = O24B-O22B
 2.19384 with sigma of 0.04
 N13-O19 \\sim N13-O20 \\sim N13-O21
 with sigma of 0.005
 N14A-O22A \\sim N14A-O23A \\sim N14A-O24A \\sim N14B-O23B \\sim N14B-O22B
\\sim N14B-O24B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N13 \\sim O19 \\sim O20 \\sim O21: within 3A with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(N14A) = Uanis(O22A) = Uanis(O23A) = Uanis(O24A) = Uanis(N14B) =
Uanis(O22B) = Uanis(O23B) = Uanis(O24B)
4. Others
 Sof(O23B)=Sof(O22B)=Sof(N14B)=Sof(O24B)=Sof(OW20)=1-FVAR(1)
 Sof(OW21)=Sof(O24A)=Sof(N14A)=Sof(O22A)=Sof(O23A)=FVAR(1)
 Fixed X: OW20(0.23718)
 Fixed Y: OW20(0.633181)
 Fixed Z: OW20(0.625641)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C14(H14),
 C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C25(H25),
  C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
 C35(H35), C36(H36), C37(H37), C38(H38), C42(H42), C43(H43), C44(H44), C45(H45),
  C48(H48), C49(H49), C50(H50), C51(H51), C54(H54), C55(H55), C56(H56),
 C57(H57), C58(H58), C59(H59), C60(H60), C61(H61), C65(H65), C66(H66), C67(H67),
  C68(H68)
5.b Idealised Me refined as rotating group:
 C70(H70A,H70B,H70C)
;
_shelx_res_checksum              28076