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_7122462
_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
'Dy N5 O15, C27 H40.5 N68 Ni10, 4(C2 H3 N), O'
_chemical_formula_sum            'C35 H52.5 Dy N77 Ni10 O16'
_chemical_formula_weight         2557.64
_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     iterative
_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                106.086(6)
_cell_angle_beta                 91.383(6)
_cell_angle_gamma                93.738(6)
_cell_formula_units_Z            2
_cell_length_a                   11.165(2)
_cell_length_b                   19.456(4)
_cell_length_c                   23.633(5)
_cell_measurement_reflns_used    1372
_cell_measurement_temperature    173.15(2)
_cell_measurement_theta_max      21.962
_cell_measurement_theta_min      2.200
_cell_volume                     4917.4(17)
_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    'olex2.solve (Bourhis et al., 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  0.2470
_diffrn_reflns_av_unetI/netI     0.4667
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            39524
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         0.898
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.707
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_description       needle
_exptl_crystal_F_000             2551
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.596
_refine_diff_density_min         -1.151
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.847
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1273
_refine_ls_number_reflns         18320
_refine_ls_number_restraints     657
_refine_ls_restrained_S_all      0.836
_refine_ls_R_factor_all          0.3184
_refine_ls_R_factor_gt           0.0882
_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^)+(0.0709P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1777
_refine_ls_wR_factor_ref         0.2643
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4257
_reflns_number_total             18320
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc07722c2.cif
_cod_data_source_block           kj_214_0m
_cod_depositor_comments
'Adding full bibliography for 7122459--7122462.cif.'
_cod_original_cell_volume        4917.6(16)
_cod_original_formula_sum        'C35 H52.50 Dy N77 Ni10 O16'
_cod_database_code               7122462
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.497
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Ni9-N66 \\sim Ni8-N63
 with sigma of 0.02
 C23-N66 \\sim C17-N63
 with sigma of 0.02
 N77-C35 \\sim N74_$1-C29_$1
 with sigma of 0.02
 C35-C36 \\sim C29_$1-C30_$1
 with sigma of 0.02
 N77-C35 \\sim N75_$2-C31_$2
 with sigma of 0.02
 C35-C36 \\sim C31_$2-C32_$2
 with sigma of 0.02
 N49-N50 \\sim N46-N47
 with sigma of 0.02
 N50-N51 \\sim N47-N48
 with sigma of 0.02
 N49-N51 \\sim N46-N48
 with sigma of 0.02
 C24-N66 \\sim C18-N63
 with sigma of 0.02
 C24-C23 \\sim C18-C17
 with sigma of 0.02
 Ni9-C24 \\sim Ni8-C18
 with sigma of 0.02
3. Rigid bond restraints
 N66
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 N77, C35, C36
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N74, C29, C30
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 N64, C19, C20
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N75, C31, C32
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N59, C9, C10
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N31, N32, N33
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N76, C33, C34
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N52, N53, N54
 with sigma for 1-2 distances of 0.05 and sigma for 1-3 distances of 0.05
 N22, N23, N24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N61, C13, C14
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N46, N47
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 N4, N5, N6
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 N66, C23, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
N74 \\sim C29 \\sim C30: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.004
N64 \\sim C19 \\sim C20: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.004
N75 \\sim C31 \\sim C32: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.004
N31 \\sim N32 \\sim N33: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.004
N76 \\sim C33 \\sim C34: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.004
N22 \\sim N23 \\sim N24: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
N61 \\sim C13 \\sim C14: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.004
N46 \\sim N47: within 2A with sigma of 0.0001 and sigma for terminal atoms of
0.0002
Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C6) \\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(C11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C14) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C17) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N14) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N16) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N26) \\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(N27) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N29) \\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(N36) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N38) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N40) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N41) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N72) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N66) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N77) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C35) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C22) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C8) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C27) \\sim
Ueq, Uanis(C25) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of
0.002
Uanis(C5) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C28) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N24) \\sim Ueq, Uanis(N37) \\sim Ueq, Uanis(N59) \\sim Ueq, Uanis(N10)
\\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(N54) \\sim Ueq, Uanis(N46) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N47) \\sim Ueq, Uanis(N42) \\sim Ueq, Uanis(N45) \\sim Ueq, Uanis(N50)
\\sim Ueq, Uanis(N49) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C32) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(N75) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(C9) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(N17) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(N22) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(N56) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(N63) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(N68) \\sim Ueq, Uanis(N67) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(N52) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(N7) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(N62) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N48) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N34) \\sim Ueq, Uanis(N16) \\sim Ueq, Uanis(N28) \\sim Ueq, Uanis(N1)
\\sim Ueq, Uanis(N13) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(O8) \\sim Ueq, Uanis(N71) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(N4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N43) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O3) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O13) \\sim
Ueq, Uanis(N73) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(O14) \\sim Ueq,
Uanis(O9) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(N70) \\sim
Ueq, Uanis(O6) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(N72) \\sim Ueq,
Uanis(O10) \\sim Ueq, Uanis(O12) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N25) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Fixed Sof: C23(0.5) C24(0.5) H24A(0.5) H24B(0.5) H24C(0.5)
6.a Riding coordinates:
 C24(H24A,H24B,H24C)
6.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C10(H10A,
 H10B,H10C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C),
 C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C32(H32A,H32B,H32C), C30(H30A,H30B,H30C), C34(H34A,
 H34B,H34C), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              13141
_shelx_hkl_checksum              96308
_olex2_submission_special_instructions 'No special instructions were received'