A topologically unique alternating {CoGd} magnetocaloric ring.
Ojea, María José Heras; Lorusso, Giulia; Craig, Gavin A.; Wilson, Claire; Evangelisti, Marco; Murrie, Mark; Chemical communications (Cambridge, England) 53 (2017) 4799–4802; doi:10.1039/c7cc02243c

data_7119974
_publ_section_title
;
 A topologically unique alternating {CoGd} magnetocaloric ring.
;
_journal_issue                   35
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4799
_journal_page_last               4802
_journal_paper_doi               10.1039/c7cc02243c
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety         'C51 H96 Co3 Gd3 N6 O32'
_chemical_formula_sum            'C51 H96 Co3 Gd3 N6 O32'
_chemical_formula_weight         1953.87
_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_Hall           'I -4 2bw'
_space_group_name_H-M_alt        'I -4 2 d'
_symmetry_space_group_name_Hall  'I -4 2bw'
_symmetry_space_group_name_H-M   'I -4 2 d'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-03-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-03-22 deposited with the CCDC.
2017-04-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.644(3)
_cell_length_b                   26.644(3)
_cell_length_c                   27.368(3)
_cell_measurement_reflns_used    9325
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      2.36
_cell_volume                     19429(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker COLLECT'
_computing_data_reduction        'Bruker SAINT'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\f & \w scans'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            246917
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.059
_diffrn_reflns_theta_max         25.059
_diffrn_reflns_theta_min         1.839
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.583
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6183
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. 
wR2(int) was 0.0884 before and 0.0693 after correction. The Ratio
 of minimum to maximum transmission is 0.8297. The \l/2 
correction factor is 0.00150.
;
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_description       Block
_exptl_crystal_F_000             7784
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.912
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details
;
 Flack x determined using 3377 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.014(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         8610
_refine_ls_number_restraints     590
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0385P)^2^+147.2165P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0967
_reflns_Friedel_coverage         0.871
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                7530
_reflns_number_total             8610
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc02243c2.cif
_cod_data_source_block           mjh71066stv_sq
_cod_depositor_comments          'Adding full bibliography for 7119974.cif.'
_cod_original_cell_volume        19428(4)
_cod_database_code               7119974
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 C102-C101 = C107-C101
 1.51 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: C201(0.5) H20A(0.5) H20B(0.5) H20C(0.5) H20D(0.5) H20E(0.5)
 H20F(0.5)
5.a Riding coordinates:
 C202(H20C,H20D), C202(H20E,H20F)
5.b Rotating group:
 O1W(H1WA,H1WB)
5.c Ternary CH refined with riding coordinates:
 N101(H101), N102(H102), N201(H201)
5.d Secondary CH2 refined with riding coordinates:
 C201(H20A,H20B), C101(H10A,H10B), C102(H10C,H10D), C104(H10E,H10F), C105(H10G,
 H10H), C106(H10I,H10J), C107(H10K,H10L), C109(H10M,H10N), C110(H11A,H11B),
 C111(H11C,H11D), C204(H20G,H20H), C205(H20I,H20J), C206(H20K,H20L)
5.e Aromatic/amide H refined with riding coordinates:
 C3A(H3A)
5.f Idealised Me refined as rotating group:
 C1A(H1AA,H1AB,H1AC), C2AC(H2AA,H2AB,H2AC), C5A(H5AA,H5AB,H5AC), C4AC(H4AA,
 H4AB,H4AC)
5.g Idealised tetrahedral OH refined as rotating group:
 O106(H106), O111(H111), O206(H206)
;
_shelx_res_checksum              78822
_shelx_fab_checksum              72035
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'