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_7230092
_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         'C35 H41 Mn3 N5 O14'
_chemical_formula_sum            'C35 H41 Mn3 N5 O14'
_chemical_formula_weight         920.55
_chemical_name_systematic        SuperNova
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                   17.0744(3)
_cell_length_b                   20.5494(4)
_cell_length_c                   11.4918(2)
_cell_measurement_reflns_used    10560
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.7008
_cell_measurement_theta_min      2.9088
_cell_volume                     4032.11(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean 15.9784
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_details
;
  1 omega  -18.00   13.00   1.0000   17.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.2686  -99.0000 -150.0000 31

  2 omega  -15.00   20.00   1.0000   17.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.2686  -99.0000  -60.0000 35

  3 omega  -20.00    5.00   1.0000   17.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.2686  -99.0000   90.0000 25

  4 omega   -7.00   83.00   1.0000   17.0000
omega____ theta____ kappa____ phi______ frames
    -       19.4405   38.0000    0.0000 90

  5 omega   61.00   98.00   1.0000   17.0000
omega____ theta____ kappa____ phi______ frames
    -       19.4405 -178.0000 -120.0000 37

  6 omega   36.00   61.00   1.0000   17.0000
omega____ theta____ kappa____ phi______ frames
    -       19.4405  178.0000 -150.0000 25

  7 omega   -4.00   84.00   1.0000   17.0000
omega____ theta____ kappa____ phi______ frames
    -       19.4405   77.0000   60.0000 88

  8 omega   57.00   83.00   1.0000   17.0000
omega____ theta____ kappa____ phi______ frames
    -       19.4405   57.0000  120.0000 26

  9 omega  -53.00   47.00   1.0000   17.0000
omega____ theta____ kappa____ phi______ frames
    -       19.4405  -38.0000 -180.0000 100

 10 omega  -50.00   37.00   1.0000   17.0000
omega____ theta____ kappa____ phi______ frames
    -       19.4405  -57.0000  -30.0000 87
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0325170000
_diffrn_orient_matrix_UB_12      -0.0093626000
_diffrn_orient_matrix_UB_13      0.0345552000
_diffrn_orient_matrix_UB_21      0.0114203000
_diffrn_orient_matrix_UB_22      0.0330749000
_diffrn_orient_matrix_UB_23      0.0049598000
_diffrn_orient_matrix_UB_31      -0.0231723000
_diffrn_orient_matrix_UB_32      0.0031407000
_diffrn_orient_matrix_UB_33      0.0509208000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            41863
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.76
_diffrn_reflns_theta_min         2.91
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.996
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1892
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         4995
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+2.7753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.1032
_reflns_number_gt                3796
_reflns_number_total             4995
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7ra12844d2.cif
_cod_data_source_block           1-Mn3
_cod_original_cell_volume        4032.12(13)
_cod_database_code               7230092
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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, All C(H,H,H,H,H) groups
2. Restrained distances
 O7-H7
 0.85 with sigma of 0.01
 O6-H6
 0.85 with sigma of 0.01
 C18-H7
 1.875 with sigma of 0.02
 C17-H6
 1.869 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C14(H14)
3.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C)
;
_olex2_submission_special_instructions 'No special instructions were received'