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_7118969
_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 O21 P4, 5(O)'
_chemical_formula_sum            'C20 H37 Gd Mn2 N8 O28 P4'
_chemical_formula_weight         1228.59
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                90.000(5)
_cell_angle_beta                 110.190(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   26.090(5)
_cell_length_b                   14.510(5)
_cell_length_c                   12.200(5)
_cell_measurement_reflns_used    1589
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      1
_cell_volume                     4335(2)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'M2DM bruker'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR2011 (POlidori 2011)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'PILATUS DECTRIS 6M'
_diffrn_measurement_method       'Phi scan'
_diffrn_radiation_type           'synchrotron radiation'
_diffrn_radiation_wavelength     0.82653
_diffrn_reflns_av_R_equivalents  0.4237
_diffrn_reflns_av_unetI/netI     0.3079
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            24777
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        29.730
_diffrn_reflns_theta_max         31.096
_diffrn_reflns_theta_min         2.549
_diffrn_source                   'synchrotron radiation'
_exptl_absorpt_coefficient_mu    3.482
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.883
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_refine_diff_density_max         3.058
_refine_diff_density_min         -3.059
_refine_diff_density_rms         0.247
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.904
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         4318
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.904
_refine_ls_R_factor_all          0.1811
_refine_ls_R_factor_gt           0.1361
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0865P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2858
_refine_ls_wR_factor_ref         0.3221
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1874
_reflns_number_total             4318
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc02908f2.cif
_cod_data_source_block           shelxl
_cod_database_code               7118969
_shelxl_version_number           2013-2
_shelx_res_checksum              29926