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_7122460
_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
'C28 H42 N68 Ni10, 0.5(N10 O30 Y2), 4(C2 H3 N)'
_chemical_formula_sum            'C36 H54 N77 Ni10 O15 Y'
_chemical_formula_weight         2481.57
_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     dual
_audit_creation_date             2018-09-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-22 deposited with the CCDC.
2018-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                78.715(9)
_cell_angle_beta                 84.321(8)
_cell_angle_gamma                81.693(9)
_cell_formula_units_Z            1
_cell_length_a                   11.0684(12)
_cell_length_b                   14.2915(16)
_cell_length_c                   16.0071(14)
_cell_measurement_reflns_used    2452
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      62.0930
_cell_measurement_theta_min      3.8220
_cell_volume                     2450.5(4)
_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      173.15
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_unetI/netI     0.0885
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16670
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        62.799
_diffrn_reflns_theta_max         62.799
_diffrn_reflns_theta_min         3.179
_exptl_absorpt_coefficient_mu    3.552
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75298
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light green'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_description       plate
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.028
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.850
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     822
_refine_ls_number_reflns         7748
_refine_ls_number_restraints     147
_refine_ls_restrained_S_all      0.851
_refine_ls_R_factor_all          0.1195
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0601P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1177
_refine_ls_wR_factor_ref         0.1482
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3621
_reflns_number_total             7748
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc07722c2.cif
_cod_data_source_block           18206ocd19
_cod_depositor_comments
'Adding full bibliography for 7122459--7122462.cif.'
_cod_database_code               7122460
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.907
_shelx_estimated_absorpt_t_min   0.718
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N25-N27
 2.325 with sigma of 0.005
 N25-N26
 1.172 with sigma of 0.005
 N26-N27
 1.147 with sigma of 0.005
 N37-O7 = N37-O8 = N37-O9
 1.245 with sigma of 0.02
 C14-C13 = C13A-C14A
 1.52 with sigma of 0.01
3. Restrained planarity
 O7, N37, O9, O8
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
N27 \\sim N26 \\sim N25: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
N34 \\sim C13 \\sim C14 \\sim C13A \\sim C14A: within 1.7A with sigma of 0.01
and sigma for terminal atoms of 0.02
Uanis(N40A) \\sim Ueq, Uanis(C15A) \\sim Ueq, Uanis(C16A) \\sim Ueq, Uanis(C16)
\\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(N40) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O13) \\sim Ueq, Uanis(N39) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O15)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C18A) \\sim Ueq, Uanis(C17A) \\sim Ueq, Uanis(N41A) \\sim Ueq, Uanis(C18)
\\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(N41) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: N26(0.5) N27(0.5) C13(0.5) Y1(0.5) O1(0.5) O2(0.5) N35(0.5)
 O3(0.5) O5(0.5) O4(0.5) O6(0.5) N36(0.5) O7(0.5) O8(0.5) N37(0.5) O9(0.5)
 C14(0.5) H14A(0.5) H14B(0.5) H14C(0.5) C13A(0.5) C14A(0.5) H14D(0.5) H14E(0.5)
 H14F(0.5) C15(0.5) N40(0.5) C16(0.5) H16A(0.5) H16B(0.5) H16C(0.5) O10(0.5)
 O12(0.5) N38(0.5) O11(0.5) O14(0.5) O13(0.5) O15(0.5) N39(0.5) C18(0.65)
 H18A(0.65) H18B(0.65) H18C(0.65) C17A(0.35) N41(0.65) N40A(0.5) C15A(0.5)
 C16A(0.5) H16D(0.5) H16E(0.5) H16F(0.5) C17(0.65) N27A(0.5) N26A(0.5)
 C18A(0.35) H17A(0.35) H17B(0.35) H18D(0.35) N41A(0.35)
6.a Riding coordinates:
 C18A(H17A,H17B,H18D)
6.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C12(H12A,H12B,H12C), C4(H4A,H4B,H4C), C8(H8A,H8B,H8C),
 C2(H2A,H2B,H2C), C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C14A(H14D,H14E,
 H14F), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C16A(H16D,H16E,H16F)
;
_shelx_res_checksum              63966
_shelx_hkl_checksum              10317
_olex2_submission_special_instructions 'No special instructions were received'