Dodenuclear [MnLn] clusters with 2-(hydroxymethyl)pyridine: syntheses, structures, and magnetic properties.
Sun, Lei; Chen, Hui; Ma, Chengbing; Chen, Changneng; Dalton transactions (Cambridge, England : 2003) 44 (2015) 20964–20971; doi:10.1039/c5dt03130c

data_7037552
_publ_section_title
;
 Dodenuclear [MnLn] clusters with 2-(hydroxymethyl)pyridine: syntheses,
 structures, and magnetic properties.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              20964
_journal_page_last               20971
_journal_paper_doi               10.1039/c5dt03130c
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C123 H103 Gd4 Mn8 N9 O52'
_chemical_formula_weight         3607.66
_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
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_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-11-05 deposited with the CCDC.
2015-11-19 downloaded from the CCDC.
;
_cell_angle_alpha                66.290(3)
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_cell_angle_gamma                84.120(3)
_cell_formula_units_Z            1
_cell_length_a                   14.3312(6)
_cell_length_b                   14.5625(4)
_cell_length_c                   17.0155(5)
_cell_measurement_reflns_used    9649
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.6850
_cell_measurement_theta_min      4.1600
_cell_volume                     3233.9(2)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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_computing_molecular_graphics
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diamond 3.0
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_computing_publication_material
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olex2-1.2
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_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.5594
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21826
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.995
_diffrn_reflns_theta_min         3.100
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    19.954
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.852
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
The unit cell contains 1 hmpH molecules which have been treated as a diffuse
contribution to the overall scattering without specific atom positions by SQUEEZE/ PLATON.
;
_refine_diff_density_max         1.393
_refine_diff_density_min         -1.317
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.900
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     889
_refine_ls_number_reflns         11998
_refine_ls_number_restraints     122
_refine_ls_restrained_S_all      0.915
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0480P)^2^+25.4436P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1165
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10027
_reflns_number_total             11998
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03130c3.cif
_cod_data_source_block           s
_cod_database_code               7037552
_audit_block_doi                 10.5517/cc143cwh
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              36900
_shelx_hkl_checksum              22299