Increasing the nuclearity and spin ground state in a new family of ferromagnetically-coupled {Ni<sub>10</sub>} disk-like complexes bearing exclusively end-on bridging azido ligands.
Krause, Jasmin; Alexandropoulos, Dimitris I.; Carrella, Luca M.; Rentschler, Eva; Stamatatos, Theocharis C.; Chemical communications (Cambridge, England) 54 (2018) 12499–12502; doi:10.1039/c8cc07722c

data_7122461
_publ_section_title
;
 Increasing the nuclearity and spin ground state in a new family of
 ferromagnetically-coupled {Ni<sub>10</sub>} disk-like complexes bearing
 exclusively end-on bridging azido ligands.
;
_journal_issue                   88
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12499
_journal_page_last               12502
_journal_paper_doi               10.1039/c8cc07722c
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety
'N5 O15 Tb, C28 H42 N68 Ni10, 4(C2 H3 N), 2(O)'
_chemical_formula_sum            'C36 H54 N77 Ni10 O17 Tb'
_chemical_formula_weight         2583.58
_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
_audit_creation_date             2018-08-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-08-30 deposited with the CCDC.
2018-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                106.432(4)
_cell_angle_beta                 91.339(4)
_cell_angle_gamma                94.085(4)
_cell_formula_units_Z            2
_cell_length_a                   11.160(2)
_cell_length_b                   19.509(4)
_cell_length_c                   23.698(4)
_cell_measurement_reflns_used    6659
_cell_measurement_temperature    173.15(2)
_cell_measurement_theta_max      27.392
_cell_measurement_theta_min      2.183
_cell_volume                     4931.1(16)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker SMART APEX2 area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2'
_diffrn_measurement_method       '\k-geometry diffractometry'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0953
_diffrn_reflns_av_unetI/netI     0.1025
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            60571
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.599
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.661
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5215
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.1029 before and 0.0585 after correction.
The Ratio of minimum to maximum transmission is 0.6994.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_description       block
_exptl_crystal_F_000             2580
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.755
_refine_diff_density_min         -1.352
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1287
_refine_ls_number_reflns         19380
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1362
_refine_ls_R_factor_gt           0.0652
_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^)+(0.0527P)^2^+17.2013P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1353
_refine_ls_wR_factor_ref         0.1641
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10656
_reflns_number_total             19380
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc07722c2.cif
_cod_data_source_block           ren-kj-176
_cod_depositor_comments
'Adding full bibliography for 7122459--7122462.cif.'
_cod_database_code               7122461
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.741
_shelx_estimated_absorpt_t_min   0.556
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N65-C21
 1.12 with sigma of 0.01
 C21-C22
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C22) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C22) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4.a Riding coordinates:
 C22(H22A,H22B,H22C)
4.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C2(H2A,H2B,H2C), C8(H8A,H8B,H8C), C28(H28A,H28B,H28C),
 C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C24(H24A,H24B,H24C), C12(H12A,H12B,H12C),
  C35(H35A,H35B,H35C), C16(H16A,H16B,H16C), C20(H20A,H20B,H20C), C4(H4A,H4B,
 H4C), C29(H29A,H29B,H29C), C18(H18A,H18B,H18C), C31(H31A,H31B,H31C), C33(H33A,
 H33B,H33C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              58698
_shelx_hkl_checksum              62501
_olex2_submission_special_instructions 'No special instructions were received'