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_4348888
_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            'C140 H224 Mn21 N9 O95'
_chemical_formula_weight         4707.01
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/cc140s0y
_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                96.546(5)
_cell_angle_beta                 102.138(4)
_cell_angle_gamma                109.674(4)
_cell_formula_units_Z            2
_cell_length_a                   15.472(5)
_cell_length_b                   19.315(6)
_cell_length_c                   33.584(10)
_cell_measurement_reflns_used    3719
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.97
_cell_measurement_theta_min      2.53
_cell_volume                     9051(5)
_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 0.984
_diffrn_measured_fraction_theta_max 0.959
_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  0.0572
_diffrn_reflns_av_unetI/netI     0.2046
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            52837
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         1.143
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.512
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6064
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            dark-brown
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_density_meas      ?
_exptl_crystal_description       lozenge
_exptl_crystal_F_000             4824
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_platon_squeeze_details
;
;
_refine_diff_density_max         1.052
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.877
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2135
_refine_ls_number_reflns         39867
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      0.880
_refine_ls_R_factor_all          0.1729
_refine_ls_R_factor_gt           0.0723
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0478P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1407
_refine_ls_wR_factor_ref         0.1642
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16323
_reflns_number_total             39867
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5qi00013k2.cif
_cod_data_source_block           Mn21
_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_database_code               4348888
_shelx_estimated_absorpt_t_min   0.752
_shelx_estimated_absorpt_t_max   0.863
_shelxl_version_number           2013-4
_shelx_res_checksum              63313
_shelx_hkl_checksum              48220