A family of 3d metal clusters based on N‒N single bonds bridged quasi-linear trinuclear cores: the Mn analogue displaying single-molecule magnet behavior
Wang, Kai; Tang, Shen; Hu, Zhao-Bo; Zou, Hua-Hong; Wang, Xiao-Lu; Li, Yan; Zhang, Shu-Hua; Chen, Zi-Lu; Liang, Fu-Pei; RSC Advances 8 (2018) 6218–; doi:10.1039/C7RA12844D

data_7230093
_publ_section_title
;
 A family of 3d metal clusters based on N--N single bonds bridged
 quasi-linear trinuclear cores: the Mn analogue displaying single-molecule
 magnet behavior
;
_journal_issue                   12
_journal_name_full               'RSC Advances'
_journal_page_first              6218
_journal_paper_doi               10.1039/C7RA12844D
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C43 H33 N9 Ni3 O8'
_chemical_formula_sum            'C43 H33 N9 Ni3 O8'
_chemical_formula_weight         979.91
_chemical_name_systematic        SuperNova
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-07-28
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-07-29 deposited with the CCDC.
2018-02-01 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.9052(2)
_cell_length_b                   25.3476(2)
_cell_length_c                   8.99870(10)
_cell_measurement_reflns_used    3681
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      28.6832
_cell_measurement_theta_min      2.9943
_cell_volume                     4084.09(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  SuperNova
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0154
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            33538
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.00
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.436
_exptl_absorpt_correction_T_max  0.7430
_exptl_absorpt_correction_T_min  0.7066
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'brownish red'
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.920
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         3681
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0265
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+5.1113P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0703
_reflns_number_gt                3482
_reflns_number_total             3681
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7ra12844d2.cif
_cod_data_source_block           4-Ni3
_cod_database_code               7230093
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C21) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Fixed Sof: C21(0.5) H21(0.5) C23(0.5) H23(0.5) C24(0.5) H24(0.5) C25(0.5)
 H25(0.5)
4.a Riding coordinates:
 N5(N6,C21), N5(H21), C22(H22), C23(H23), C24(H24), C25(H25)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18), C19(H19), C20(H20)
4.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;
_olex2_submission_special_instructions 'No special instructions were received'