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_7122459
_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
'C14 H21 N34 Ni4.29, C14 H21 N34 Ni5, Gd0.86 N5 O15, 6(C2 H3 N), 0.14(Gd), 0.71(Ni), 2(O)'
_chemical_formula_sum            'C40 H60 Gd N79 Ni10 O17'
_chemical_formula_weight         2664.02
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-08-28
_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                105.722(4)
_cell_angle_beta                 93.827(4)
_cell_angle_gamma                103.427(4)
_cell_formula_units_Z            2
_cell_length_a                   11.1561(16)
_cell_length_b                   17.898(3)
_cell_length_c                   28.868(4)
_cell_measurement_reflns_used    8037
_cell_measurement_temperature    173.15(2)
_cell_measurement_theta_max      27.012
_cell_measurement_theta_min      2.182
_cell_volume                     5344.8(14)
_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)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1057
_diffrn_reflns_av_unetI/netI     0.1652
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            47462
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         0.740
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.417
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5367
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.1002 before and 0.0582 after correction.
The Ratio of minimum to maximum transmission is 0.7198.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_description       block
_exptl_crystal_F_000             2666
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.359
_refine_diff_density_min         -2.081
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1369
_refine_ls_number_reflns         20931
_refine_ls_number_restraints     196
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.2260
_refine_ls_R_factor_gt           0.1433
_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^)+(0.0001P)^2^+282.1843P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2949
_refine_ls_wR_factor_ref         0.3313
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10919
_reflns_number_total             20931
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc07722c2.cif
_cod_data_source_block           kj_200_gd_0m
_cod_depositor_comments
'Adding full bibliography for 7122459--7122462.cif.'
_cod_original_cell_volume        5344.8(13)
_cod_database_code               7122459
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.760
_shelx_estimated_absorpt_t_min   0.583
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N75-C31
 2.6 with sigma of 0.02
 N74-C29
 2.6 with sigma of 0.02
 N80-C41
 2.6 with sigma of 0.02
 N77-C35
 2.6 with sigma of 0.02
 N78-C37
 2.6 with sigma of 0.02
 N79-C39
 2.6 with sigma of 0.02
 N69-O1
 1.25 with sigma of 0.02
3. Rigid bond restraints
 N7, N8, N9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 N31, C7, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 N30, C5, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C5)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N7) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(N10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N35) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N47) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N59) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N58) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N73) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O9) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O6) \\sim Ueq, Uanis(N70) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Ni3) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(N74) \\sim Ueq, Uanis(N75) \\sim Ueq, Uanis(N24) \\sim Ueq, Uanis(N23)
\\sim Ueq, Uanis(N18) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C8) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C12) \\sim
Ueq, Uanis(C32) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C36) \\sim Ueq: with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O16) \\sim Ueq, Uanis(O17) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Sof(Gd0A)=Sof(Ni1A)=Sof(Ni2A)=Sof(Ni3A)=Sof(Ni4A)=Sof(Ni5A)=1-FVAR(1)
 Sof(Ni5)=Sof(Ni4)=Sof(Ni1)=Sof(Ni3)=Sof(Ni2)=Sof(Gd1)=FVAR(1)
6.a Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C12(H12A,H12B,H12C), C10(H10A,H10B,H10C), C8(H8A,H8B,
 H8C), C6(H6A,H6B,H6C), C4(H4A,H4B,H4C), C2(H2A,H2B,H2C), C16(H16A,H16B,H16C),
 C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C37(H37A,H37B,H37C), C29(H29A,
 H29B,H29C), C41(H41A,H41B,H41C), C35(H35A,H35B,H35C), C39(H39A,H39B,H39C),
 C31(H31A,H31B,H31C)
;
_shelx_res_checksum              41358
_shelx_hkl_checksum              31738
_olex2_submission_special_instructions 'No special instructions were received'