Cluster-based networks: assembly of a (4,4) layer and a rare T-shaped bilayer from [MnIII2MnII4O2(RCOO)10] coordination clusters
Malaestean, Iurie L.; Ellern, Arkady; van Leusen, Jan; Kravtsov, Victor C.; Kögerler, Paul; Baca, Svetlana G.; CrystEngComm 16 (2014) 6523–; doi:10.1039/c4ce00504j

data_7216411
_publ_section_title
;
 Cluster-based networks: assembly of a (4,4) layer and a rare T-shaped
 bilayer from [MnIII2MnII4O2(RCOO)10] coordination clusters
;
_journal_issue                   29
_journal_name_full               CrystEngComm
_journal_page_first              6523
_journal_paper_doi               10.1039/c4ce00504j
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C62 H102 Mn6 N4 O24'
_chemical_formula_weight         1617.12
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.960(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.933(3)
_cell_length_b                   18.5408(16)
_cell_length_c                   22.9605(17)
_cell_measurement_reflns_used    3394
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.7518
_cell_measurement_theta_min      2.9089
_cell_volume                     9635.7(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 15.9914
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_sigmaI/netI    0.2008
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13185
_diffrn_reflns_theta_full        24.15
_diffrn_reflns_theta_max         24.15
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    0.820
_exptl_absorpt_correction_T_max  0.9009
_exptl_absorpt_correction_T_min  0.7142
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.115
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prizm
_exptl_crystal_F_000             3376
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_platon_squeeze_details
;
Two huge squeeze voids of 1372 and 1372A3 were found in crystal
lattice of 1, therefore SQUEEZE was used to treat traces of diffuses
solvent in those voids. There was no any electron density on difference
Fourier synthesis before SQUEEZE procedure which could be identified
as solvent. Only 9.0 and 9.1 uncounted electrons of diffused electron
density were found in these voids. Such electron density corresponds
approximately to one water molecule per one void. For non centrosymmetric
C-centered monoclinic unit sell it is corresponds to 0.5H2O molecule per
cluster. Taking in account that these voids much bigger then it is 
necessary for single water molecule and another solvents such as MeCN or EtOH,
which have been used in synthesis of crystal as well their mixture may also 
occupy such huge cavities. The UNIT instruction was not corrected for diffused
solvent molecules, because it is impossible to identify them. 
Another six squeeze voids are equal or less than 14 A3 each and contain
negligible uncounted electrons (less than 0.7).
;
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     866
_refine_ls_number_reflns         12141
_refine_ls_number_restraints     918
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1807
_refine_ls_R_factor_gt           0.0766
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0807P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1664
_refine_ls_wR_factor_ref         0.1876
_reflns_number_gt                5439
_reflns_number_total             12141
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce00504j2.cif
_cod_data_source_block           v_34_d36b1_sq
_cod_depositor_comments
'Adding full bibliography for 7216411--7216413.cif.'
_cod_original_cell_volume        9635.8(17)
_cod_original_sg_symbol_H-M      C2
_cod_database_code               7216411