A novel oxalate-based three-dimensional coordination polymer showing magnetic ordering and high proton conductivity
Mon, Marta; Vallejo, Julia; Pasán, Jorge; Fabelo, Oscar; Train, Cyrille; Verdaguer, Michel; Ohkoshi, Shin-ichi; Tokoro, Hiroko; Nakagawa, Kosuke; Pardo, Emilio; Dalton Trans.  (2017) –; doi:10.1039/C7DT03415F

data_7044446
_publ_section_title
;
 A novel oxalate-based three-dimensional coordination polymer showing
 magnetic ordering and high proton conductivity
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03415F
_journal_year                    2017
_chemical_formula_sum            'C48 H42 Cr4 Mn2 N16 O49'
_chemical_formula_weight         1944.85
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           179
_space_group_name_Hall           'P 65 2 (0 0 1)'
_space_group_name_H-M_alt        'P 65 2 2'
_symmetry_space_group_name_Hall  'P 65 2 (0 0 1)'
_symmetry_space_group_name_H-M   'P 65 2 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2017-06-12 deposited with the CCDC.
2017-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   18.80530(10)
_cell_length_b                   18.80530(10)
_cell_length_c                   43.3432(4)
_cell_measurement_reflns_used    45362
_cell_measurement_temperature    45(2)
_cell_measurement_theta_max      25.6510
_cell_measurement_theta_min      1.4620
_cell_volume                     13274.32(16)
_computing_cell_refinement       'CrysAlis PRO software program'
_computing_data_collection       'CrysAlis PRO software program'
_computing_data_reduction        'CrysAlis PRO software program'
_computing_molecular_graphics    'Mercury (McRae, 2006)'
_computing_publication_material  'WINGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      45(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.66910
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.0133
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            137416
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        23.669
_diffrn_reflns_theta_max         23.766
_diffrn_reflns_theta_min         1.472
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.718
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            dark-blue
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_description       prism
_exptl_crystal_F_000             5880
_exptl_crystal_preparation       ', Magnetic properties,Proton conductivity'
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.08(3)
_refine_ls_extinction_coef       0.0031(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         8076
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0540
_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^)+(0.1287P)^2^+4.2713P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1728
_refine_ls_wR_factor_ref         0.1765
_reflns_Friedel_coverage         0.720
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                7646
_reflns_number_total             8076
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03415f2.cif
_cod_data_source_block           shelx_CCDC1
_cod_original_cell_volume        13274.30(19)
_cod_database_code               7044446
_shelx_estimated_absorpt_t_min   0.936
_shelx_estimated_absorpt_t_max   0.936
_shelxl_version_number           2014-3
_shelx_res_checksum              61610
_shelx_fab_checksum              1485