Syntheses, structures and magnetism of mixed-valence Mn19 and Mn21 complexes supported by alkylamine-based alkoxo-bridging ligands
Ida, Hiromichi; Shiga, Takuya; Newton, Graham N.; Oshio, Hiroki; Inorganic Chemistry Frontiers 2 (2015) 538–; doi:10.1039/C5QI00013K

data_4348887
_publ_section_title
;
 Syntheses, structures and magnetism of mixed-valence Mn19 and Mn21
 complexes supported by alkylamine-based alkoxo-bridging ligands
;
_journal_issue                   6
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              538
_journal_paper_doi               10.1039/C5QI00013K
_journal_volume                  2
_journal_year                    2015
_chemical_formula_sum            'C150 H182 Cl2 Mn19 N4 O80'
_chemical_formula_weight         4435.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/cc140rzw
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-01-14 deposited with the CCDC.
2015-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.033(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   35.738(7)
_cell_length_b                   19.551(4)
_cell_length_c                   25.253(5)
_cell_measurement_reflns_used    6348
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.84
_cell_measurement_theta_min      2.24
_cell_volume                     17426(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0941
_diffrn_reflns_av_unetI/netI     0.1513
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            48768
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         1.154
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.452
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6513
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            dark-brown
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_density_meas      ?
_exptl_crystal_description       lozenge
_exptl_crystal_F_000             9036
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_platon_squeeze_details
;
;
_refine_diff_density_max         1.108
_refine_diff_density_min         -0.828
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1109
_refine_ls_number_reflns         19850
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1566
_refine_ls_R_factor_gt           0.0760
_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^)+(0.0908P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1705
_refine_ls_wR_factor_ref         0.1975
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10921
_reflns_number_total             19850
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5qi00013k2.cif
_cod_data_source_block           Mn19
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4348887
_shelx_estimated_absorpt_t_min   0.868
_shelx_estimated_absorpt_t_max   0.944
_shelxl_version_number           2013-4
_shelx_res_checksum              65569
_shelx_hkl_checksum              49297