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_7055384
_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 Gd N12 O18, 2(N O3), 20(H2 O)'
_chemical_formula_sum            'C70 H91 Cr4 Gd N14 O44'
_chemical_formula_weight         2197.81
_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
_audit_creation_date             2015-12-01
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-12-04 deposited with the CCDC.
2016-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.8109(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.81501(17)
_cell_length_b                   24.2384(2)
_cell_length_c                   22.06575(19)
_cell_measurement_reflns_used    57262
_cell_measurement_temperature    183(1)
_cell_measurement_theta_max      74.4
_cell_measurement_theta_min      1.9
_cell_volume                     8947.10(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      183(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  1  \w    -96.00  -2.00   1.00    5.00    --  -41.82 125.00-180.00   94
  2  \w   -115.00 -14.00   1.00    5.00    --  -41.82 -57.00  60.00  101
  3  \w    -66.00  33.00   1.00    5.00    --  -41.82  37.00-150.00   99
  4  \w     40.00 141.00   1.00   20.00    --  112.00 -61.00   0.00  101
  5  \w     39.00 138.00   1.00   20.00    --  112.00 -45.00-150.00   99
  6  \w     36.00 145.00   1.00   20.00    --  112.00 -77.00 -60.00  109
  7  \w     39.00 138.00   1.00   20.00    --  112.00 -45.00   0.00   99
  8  \w    100.00 178.00   1.00   20.00    --  112.00 111.00 -90.00   78
  9  \w     59.00 178.00   1.00   20.00    --  112.00  15.00  60.00  119
 10  \w     40.00 141.00   1.00   20.00    --  112.00 -61.00-180.00  101
 11  \w     36.00 140.00   1.00   20.00    --  112.00 -30.00 150.00  104
 12  \w     83.00 178.00   1.00   20.00    --  112.00  61.00 150.00   95
 13  \w     36.00 145.00   1.00   20.00    --  112.00 -77.00-150.00  109
 14  \w   -116.00 -17.00   1.00    5.00    --  -41.82 -37.00-150.00   99
 15  \w   -115.00 -14.00   1.00    5.00    --  -41.82 -57.00 -30.00  101
 16  \w   -115.00 -14.00   1.00    5.00    --  -41.82 -57.00 150.00  101
 17  \w   -118.00 -27.00   1.00    5.00    --  -41.82 -77.00 -90.00   91
 18  \w      1.00  83.00   1.00    5.00    --   41.82 -99.00  30.00   82
 19  \f     30.00 300.00   1.00    0.50   0.00   0.00   0.00    --   270
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0864628000
_diffrn_orient_matrix_UB_12      -0.0058876000
_diffrn_orient_matrix_UB_13      -0.0299393000
_diffrn_orient_matrix_UB_21      -0.0250163000
_diffrn_orient_matrix_UB_22      -0.0253041000
_diffrn_orient_matrix_UB_23      0.0592566000
_diffrn_orient_matrix_UB_31      -0.0198303000
_diffrn_orient_matrix_UB_32      0.0579547000
_diffrn_orient_matrix_UB_33      0.0227263000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            94437
_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         74.489
_diffrn_reflns_theta_min         2.716
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.494
_exptl_absorpt_correction_T_max  0.695
_exptl_absorpt_correction_T_min  0.188
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_description       plate
_exptl_crystal_F_000             4484
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.280
_refine_diff_density_min         -0.924
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1205
_refine_ls_number_reflns         18265
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0684P)^2^+25.0040P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1247
_refine_ls_wR_factor_ref         0.1347
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15526
_reflns_number_total             18265
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj00136j2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7055381--7055384.cif.'
_cod_database_code               7055384
_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
 N13B-O45B \\sim N13B-O43 \\sim N13B-O44B \\sim N13A-O43 \\sim N13A-O45A \\sim
N13A-O44A
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(O45A) = Uanis(N13A) = Uanis(O45B) = Uanis(N13B) = Uanis(O44B) = Uanis(O43)
4. Rigid body (RIGU) restrains
 O43, O44B, O45B, N13B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O40, O41, O42, N14
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O43, O44B, O45B, N13B, O44A, O45A, N13A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Fixed Sof: O44B(0.75) O45B(0.75) N13B(0.75) O44A(0.25) O45A(0.25) N13A(0.25)
 O33(0.75) O34(0.75) O38(0.75) O32(0.75)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22), C23(H23),
  C25(H25), C26(H26), C27(H27), C28(H28), C31(H31), C32(H32), C33(H33),
 C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42),
  C43(H43), C46(H46), C47(H47), C48(H48), C49(H49), C54(H54), C55(H55),
 C56(H56), C57(H57), C59(H59), C60(H60), C61(H61), C62(H62), C65(H65), C66(H66),
  C67(H67), C68(H68)
6.b Idealised Me refined as rotating group:
 C70(H70A,H70B,H70C)
;
_shelx_res_checksum              59465
_shelx_shelxl_version_number     2014/7