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_7055381
_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), 19(H2 O)'
_chemical_formula_sum            'C70 H89 Cr4 Dy N14 O43'
_chemical_formula_weight         2185.05
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_audit_creation_date             2014-04-24
_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                80.244(2)
_cell_angle_beta                 82.550(2)
_cell_angle_gamma                85.849(2)
_cell_formula_units_Z            2
_cell_length_a                   12.3890(3)
_cell_length_b                   17.8502(4)
_cell_length_c                   20.4246(5)
_cell_measurement_reflns_used    21940
_cell_measurement_temperature    183(1)
_cell_measurement_theta_max      32.8
_cell_measurement_theta_min      2.3
_cell_volume                     4408.04(18)
_computing_cell_refinement
;
CrysAlisPro, version 1.171.37.31 (Agilent Technologies, 2012)
;
_computing_data_collection
;
CrysAlisPro, version 1.171.37.31 (Agilent Technologies, 2012)
;
_computing_data_reduction
;
CrysAlisPro, version 1.171.36.20 (Agilent Technologies, 2012)
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_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 10.4498
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0340182000
_diffrn_orient_matrix_UB_12      0.0271369000
_diffrn_orient_matrix_UB_13      -0.0205410000
_diffrn_orient_matrix_UB_21      -0.0452466000
_diffrn_orient_matrix_UB_22      0.0266057000
_diffrn_orient_matrix_UB_23      -0.0025329000
_diffrn_orient_matrix_UB_31      0.0117602000
_diffrn_orient_matrix_UB_32      0.0136273000
_diffrn_orient_matrix_UB_33      0.0288320000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0754
_diffrn_reflns_av_unetI/netI     0.0795
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            108656
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.470
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.418
_exptl_absorpt_correction_T_max  0.926
_exptl_absorpt_correction_T_min  0.758
_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            violet
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_description       plate
_exptl_crystal_F_000             2226
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.475
_refine_diff_density_min         -0.956
_refine_diff_density_rms         0.131
_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     1139
_refine_ls_number_reflns         26897
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0412P)^2^+2.5117P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1145
_reflns_number_gt                19940
_reflns_number_total             26897
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj00136j2.cif
_cod_data_source_block           1a
_cod_depositor_comments
'Adding full bibliography for 7055381--7055384.cif.'
_cod_original_cell_volume        4408.06(19)
_cod_database_code               7055381
_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, All O(H,H) groups
2.a Free rotating group:
 OW1(HW1A,HW1B,OW2,HW2A,HW2B,OW3,HW3A,HW3B,OW4,HW4A,HW4B,OW5,HW5A,HW5B,OW6,
 HW6A,HW6B,OW7,HW7A,HW7B,OW8,HW8A,HW8B,OW9,HW9A,HW9B,OW10,HW1C,HW1D,OW11,HW1E,
 HW1F,OW12,HW1G,HW1H,OW13,HW1I,HW1J,OW14,HW1K,HW1L,OW15,HW1M,HW1N,OW16,HW1O,
 HW1P,OW17,HW1Q,HW1R,OW18,HW1S,HW1T,OW19,HW1U,HW1V)
2.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)
2.c Idealised Me refined as rotating group:
 C70(H70A,H70B,H70C)
;
_shelx_res_checksum              16383