Controllable formation of heterotrimetallic coordination compounds: systematically incorporating lanthanide and alkali metal ions into the manganese 12-metallacrown-4 framework.
Azar, Michael R.; Boron, 3rd, Thaddeus T; Lutter, Jacob C.; Daly, Connor I.; Zegalia, Kelcie A.; Nimthong, Ruthairat; Ferrence, Gregory M.; Zeller, Matthias; Kampf, Jeff W.; Pecoraro, Vincent L.; Zaleski, Curtis M.; Inorganic chemistry 53 (2014) 1729–1742; doi:10.1021/ic402865p

data_4337608
_publ_section_title
;
 Controllable formation of heterotrimetallic coordination compounds:
 systematically incorporating lanthanide and alkali metal ions into the
 manganese 12-metallacrown-4 framework.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1729
_journal_page_last               1742
_journal_paper_doi               10.1021/ic402865p
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C36 H36 Mn4 N4 Na O24 Y,6(C3 H7 N O)'
_chemical_formula_sum            'C54 H78 Mn4 N10 Na O30 Y'
_chemical_formula_weight         1678.92
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                89.4150(10)
_cell_angle_beta                 88.8920(10)
_cell_angle_gamma                73.1890(10)
_cell_formula_units_Z            2
_cell_length_a                   12.9998(10)
_cell_length_b                   16.0840(12)
_cell_length_c                   17.3773(13)
_cell_measurement_reflns_used    9573
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.3027
_cell_measurement_theta_min      2.3445
_cell_volume                     3477.4(5)
_computing_cell_refinement       'SAINT V8.18C (Bruker, 2012)'
_computing_data_collection       'Apex2 v2012.4-3 (Bruker, 2012)'
_computing_data_reduction        'SAINT V8.18C (Bruker, 2012)'
_computing_molecular_graphics    'Shelxtl (Bruker, 2003)'
_computing_publication_material  'Shelxtl (Bruker, 2003)'
_computing_structure_refinement
;  
SHELXL-2013 (Sheldrick, 2013), 
SHELXLE Rev609 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Bruker AXS SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            161036
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.326
_diffrn_reflns_theta_min         2.152
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    1.630
_exptl_absorpt_correction_T_max  0.746036
_exptl_absorpt_correction_T_min  0.500083
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2009)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_description       plate
_exptl_crystal_F_000             1724
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.921
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details
;
 Flack x determined using 14420 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.236(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1319
_refine_ls_number_reflns         56304
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+2.0051P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.0996
_reflns_Friedel_coverage         0.896
_reflns_Friedel_fraction_full    0.935
_reflns_Friedel_fraction_max     0.852
_reflns_number_gt                47484
_reflns_number_total             56304
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic402865p_si_001.cif
_cod_data_source_block           12_13mz171_0m
_cod_database_code               4337608
_shelx_estimated_absorpt_t_min   0.562
_shelx_estimated_absorpt_t_max   0.923
_shelxl_version_number           2012-9
_shelx_res_checksum              21654
_shelx_hkl_checksum              59217