Cationic Mn 2+ /H + exchange leading a slow solid-state transformation of a 2D porphyrinic network at ambient conditions
Amayuelas, Eder; Fidalgo-Marijuan, Arkaitz; Bazán, Begoña; Urtiaga, Miren Karmele; Barandika, Gotzone; Lezama, Luis; Arriortua, María Isabel; Journal of Solid State Chemistry 247 (2017) 161–167; doi:10.1016/j.jssc.2017.01.012

data_1560619
_publ_section_title
;
 Cationic Mn 2+ /H + exchange leading a slow solid-state transformation of
 a 2D porphyrinic network at ambient conditions
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              161
_journal_page_last               167
_journal_paper_doi               10.1016/j.jssc.2017.01.012
_journal_volume                  247
_journal_year                    2017
_chemical_formula_moiety         '0.5(C96 H48 Mn6 N8 O26)'
_chemical_formula_sum            'C48 H24 Mn3 N4 O13'
_chemical_formula_weight         1029.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_Int_Tables_number      12
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 106.842(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.6713(16)
_cell_length_b                   23.7434(19)
_cell_length_c                   9.9624(7)
_cell_measurement_reflns_used    171
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      41.0594
_cell_measurement_theta_min      2.9586
_cell_measurement_wavelength     1.54184
_cell_volume                     4453.5(6)
_computing_cell_refinement
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 5.2012
_diffrn_measured_fraction_theta_full 0.897
_diffrn_measured_fraction_theta_max 0.897
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0253635
_diffrn_orient_matrix_UB_12      -0.0480399
_diffrn_orient_matrix_UB_13      -0.0538726
_diffrn_orient_matrix_UB_21      -0.1548281
_diffrn_orient_matrix_UB_22      0.011106
_diffrn_orient_matrix_UB_23      -0.0120911
_diffrn_orient_matrix_UB_31      0.0127387
_diffrn_orient_matrix_UB_32      0.0420799
_diffrn_orient_matrix_UB_33      -0.0584813
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     1.0117
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6023
_diffrn_reflns_theta_full        65
_diffrn_reflns_theta_max         65
_diffrn_reflns_theta_min         3
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.717
_exptl_absorpt_correction_T_max  0.918
_exptl_absorpt_correction_T_min  0.808
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
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        CrysAlisPro, Agilent Technologies,
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Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    0.7677
_exptl_crystal_density_meas      1.346(5)
_exptl_crystal_density_method    Flotation
_exptl_crystal_description       prism
_exptl_crystal_F_000             1038.1926
_exptl_crystal_size_max          0.1607
_exptl_crystal_size_mid          0.0874
_exptl_crystal_size_min          0.0527
_refine_diff_density_max         1.2461
_refine_diff_density_min         -1.3679
_refine_diff_density_rms         0.1067
_refine_ls_goodness_of_fit_ref   1.0002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    19
_refine_ls_number_parameters     183
_refine_ls_number_reflns         3493
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      0.9964
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0798
_refine_ls_shift/su_max          0.0004
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1889P)^2^+3.0168P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2458
_refine_ls_wR_factor_ref         0.2677
_reflns_number_gt                2407
_reflns_number_total             3493
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            JSSC-2017-247-161.cif
_cod_data_source_block           ea113
_cod_database_code               1560619