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_7055382
_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 Dy N12 O18, 2(N O3), 20(H2 O)'
_chemical_formula_sum            'C70 H91 Cr4 Dy N14 O44'
_chemical_formula_weight         2203.06
_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     heavy
_audit_creation_date             2014-04-28
_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                 95.739(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7984(3)
_cell_length_b                   24.1625(4)
_cell_length_c                   22.0725(4)
_cell_measurement_reflns_used    39552
_cell_measurement_temperature    183(1)
_cell_measurement_theta_max      32.9
_cell_measurement_theta_min      2.2
_cell_volume                     8914.1(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                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1900
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0319947000
_diffrn_orient_matrix_UB_12      0.0052512000
_diffrn_orient_matrix_UB_13      -0.0227542000
_diffrn_orient_matrix_UB_21      0.0229277000
_diffrn_orient_matrix_UB_22      0.0210435000
_diffrn_orient_matrix_UB_23      -0.0124167000
_diffrn_orient_matrix_UB_31      0.0158973000
_diffrn_orient_matrix_UB_32      -0.0197836000
_diffrn_orient_matrix_UB_33      -0.0192476000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0822
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            217701
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.227
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.404
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.750
_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    1.642
_exptl_crystal_description       needle
_exptl_crystal_F_000             4492
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.969
_refine_diff_density_min         -1.506
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1159
_refine_ls_number_reflns         27196
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0504
_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^)+(0.0568P)^2^+22.8005P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1237
_refine_ls_wR_factor_ref         0.1374
_reflns_number_gt                20415
_reflns_number_total             27196
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj00136j2.cif
_cod_data_source_block           1b
_cod_depositor_comments
'Adding full bibliography for 7055381--7055384.cif.'
_cod_database_code               7055382
_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
 2.23228 with sigma of 0.04
 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(OW19)=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 Free rotating group:
 OW4(OW6,OW9,OW11,OW13,OW17,OW10,OW3,OW5,OW16,OW1,OW8,OW7,OW19,OW15,OW2)
5.b 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.c Idealised Me refined as rotating group:
 C70(H70A,H70B,H70C)
;
_shelx_res_checksum              65182