Temperature- and pressure-induced phase transitions in the niccolite-type formate framework of [H3N(CH3)4NH3][Mn2(HCOO)6]
Miroslaw Maczka; Anna Gagor; Nathalia Leal Marinho Costa; Waldeci Paraguassu; Adam Sieradzki; Adam Pikul; Journal of Materials Chemistry C 4 (2016) 3185–3194; doi:10.1039/C6TC00611F

data_7234661
_publ_section_title
;
 Temperature- and pressure-induced phase transitions in the niccolite-type
 formate framework of [H3N(CH3)4NH3][Mn2(HCOO)6]
;
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              3185
_journal_page_last               3194
_journal_paper_doi               10.1039/C6TC00611F
_journal_volume                  4
_journal_year                    2016
_chemical_formula_sum            'C10 H20 Mn2 N2 O12'
_chemical_formula_weight         470.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90.060(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5477(2)
_cell_length_b                   15.2820(3)
_cell_length_c                   13.6085(3)
_cell_measurement_reflns_used    6099
_cell_measurement_temperature    90.0(4)
_cell_measurement_theta_max      29.2120
_cell_measurement_theta_min      2.6640
_cell_volume                     1777.62(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      90.0(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.874
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.874
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10570
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.874
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         29.551
_diffrn_reflns_theta_min         2.666
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.484
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90922
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_description       prism
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.404(19)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         3860
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0255
_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^)+(0.0220P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0539
_refine_ls_wR_factor_ref         0.0554
_reflns_Friedel_coverage         0.996
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.874
_reflns_number_gt                3638
_reflns_number_total             3860
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            J-Mater-Chem-C-2016-4-3185.cif
_cod_data_source_block           90K
_cod_original_cell_volume        1777.61(7)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7234661
_oxdiff_exptl_absorpt_empirical_full_min 0.905
_oxdiff_exptl_absorpt_empirical_full_max 1.113
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              29276
_shelx_hkl_checksum              18582