Ligand-Based Phase Control in Porous Molecular Assemblies.
Barreda, Omar; Bannwart, Gianluca; Yap, Glenn P. A.; Bloch, Eric D.; ACS applied materials & interfaces 10 (2018) 11420–11424; doi:10.1021/acsami.8b02015

data_4515375
_publ_section_title
;
 Ligand-Based Phase Control in Porous Molecular Assemblies.
;
_journal_issue                   14
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_page_first              11420
_journal_page_last               11424
_journal_paper_doi               10.1021/acsami.8b02015
_journal_volume                  10
_journal_year                    2018
_chemical_formula_sum            'C18.5 H7 Cu2 O12'
_chemical_formula_weight         548.32
_space_group_crystal_system      tetragonal
_space_group_IT_number           104
_space_group_name_Hall           'P 4 -2n'
_space_group_name_H-M_alt        'P 4 n c'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   26.7770(6)
_cell_length_b                   26.7770(6)
_cell_length_c                   18.7751(6)
_cell_measurement_reflns_used    9855
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      50.42
_cell_measurement_theta_min      2.87
_cell_volume                     13461.9(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker AXS APEX diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0746
_diffrn_reflns_av_unetI/netI     0.0586
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            94062
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        50.545
_diffrn_reflns_theta_max         50.545
_diffrn_reflns_theta_min         2.874
_exptl_absorpt_coefficient_mu    1.932
_exptl_absorpt_correction_T_max  0.7500
_exptl_absorpt_correction_T_min  0.6389
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'APEX3 (Bruker, 2015)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.082
_exptl_crystal_description       block
_exptl_crystal_F_000             4352
_exptl_crystal_size_max          0.142
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.123
_refine_diff_density_max         2.195
_refine_diff_density_min         -1.241
_refine_diff_density_rms         0.206
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.42(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.634
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         6987
_refine_ls_number_restraints     973
_refine_ls_restrained_S_all      1.586
_refine_ls_R_factor_all          0.1418
_refine_ls_R_factor_gt           0.1291
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3419
_refine_ls_wR_factor_ref         0.3679
_reflns_Friedel_coverage         0.926
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                5901
_reflns_number_total             6987
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am8b02015_si_009.cif
_cod_data_source_block           eric051_sq
_cod_original_cell_volume        13461.9(7)
_cod_original_formula_sum        'C18.50 H7 Cu2 O12'
_cod_database_code               4515375
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.771
_shelx_estimated_absorpt_t_max   0.797
_shelx_res_checksum              95404
_shelx_hkl_checksum              82408
_shelx_fab_checksum              22387