Single-crystal and humidity-controlled powder diffraction study of the breathing effect in a metal-organic framework upon water adsorption/desorption
Javier Arinez-Soriano; Jorge Albalad; Christian Vila-Parrondo; Javier Perez-Carvajal; Sabina Rodriguez-Hermida; Aurelio Cabeza; Jordi Juanhuix; Inhar Imaz; Daniel Maspoch; Chem.Commun. 52 (2016) 7229–; doi:10.1039/C6CC02908F

data_7118968
_publ_section_title
;
 Single-crystal and humidity-controlled powder diffraction study of the
 breathing effect in a metal-organic framework upon water
 adsorption/desorption
;
_journal_name_full               Chem.Commun.
_journal_page_first              7229
_journal_paper_doi               10.1039/C6CC02908F
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C20 H37 Gd Mn2 N8 O44 P4, 21(O)'
_chemical_formula_sum            'C20 H37 Gd Mn2 N8 O44 P4'
_chemical_formula_weight         1484.58
_chemical_name_common            1-op
_chemical_name_systematic        '[Mn2(Gd-H-DOTA-4AmP)(H2O)7].21H2O '
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-03-29 deposited with the CCDC.
2016-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.30(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.300(5)
_cell_length_b                   19.750(5)
_cell_length_c                   24.630(5)
_cell_measurement_reflns_used    2638
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50
_cell_measurement_theta_min      1
_cell_volume                     5958(3)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.789
_diffrn_measurement_device_type  synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.88557
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_unetI/netI     0.0689
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.789
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            31272
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.789
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         32.487
_diffrn_reflns_theta_min         1.650
_exptl_absorpt_coefficient_mu    3.111
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_description       prism
_exptl_crystal_F_000             2956
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         4.682
_refine_diff_density_min         -1.056
_refine_diff_density_rms         0.253
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         8782
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0876
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1429P)^2^+55.6841P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2453
_refine_ls_wR_factor_ref         0.2481
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8049
_reflns_number_total             8782
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc02908f2.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        5957.7(15)
_cod_database_code               7118968
_shelxl_version_number           2013-3
_shelx_res_checksum              78096