Metal removal from the secondary building unit of bio-MOF-1 by adenine N6-alkylation while retaining the overall 3D porous topology
Garcia-Raso, Angel; TERRON, ANGEL; rosello, Yannick; Frontera, Antonio; Castillo, Oscar; Beobide, Garikoitz; Perez-Yañez, Sonia; Escudero, Eduardo Carmelo; FIOL, JUAN J J; CrystEngComm  (2020) –; doi:10.1039/D0CE00631A

data_7240497
_publ_section_title
;
 Metal removal from the secondary building unit of bio-MOF-1 by adenine
 N6-alkylation while retaining the overall 3D porous topology
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00631A
_journal_year                    2020
_chemical_formula_iupac
(C2H8N)2[Zn6(O)(C9H12N5)4(C14H8O4)4]\^A.4(C3H7NO)\^A.13(H2O)
_chemical_formula_moiety
'2(C2 H8 N), C92 H80 N20 O17 Zn6, 4(C3 H7 N O), 13(H2 O)'
_chemical_formula_sum            'C108 H150 N26 O34 Zn6'
_chemical_formula_weight         2748.75
_chemical_name_systematic
'poly-{(dimethylammonium) [tetrakis(mu3-butyladeninato-kN3:kN7:kN9)tetrakis(mu-biphenyldicarboxylato-kO:kO')(mu4-oxido)hexazincate]-dimethylformamide-water (1/4/13)'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           48
_space_group_name_Hall           '-P 2ab 2bc'
_space_group_name_H-M_alt        'P n n n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_audit_update_record
;
2020-03-22 deposited with the CCDC.	2020-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.7914(11)
_cell_length_b                   25.4192(11)
_cell_length_c                   26.4883(8)
_cell_measurement_reflns_used    53516
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.358
_cell_measurement_theta_min      2.252
_cell_measurement_wavelength     0.71073
_cell_volume                     13999.1(10)
_computing_cell_refinement       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2003)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Sir92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  '1/4chi goniometer'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans
;
_diffrn_measurement_specimen_support 'magnetic support with MicroMount'
_diffrn_radiation_monochromator  'Confocal Max Flux optic'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0758
_diffrn_reflns_av_unetI/netI     0.0711
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            53516
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.358
_diffrn_reflns_theta_min         2.252
_diffrn_source                   'Microfocus rotating anode X-ray tube'
_diffrn_source_current           24
_diffrn_source_power             50
_diffrn_source_size              '0.2 mm x 0.2 mm fine focus'
_diffrn_source_type              'Rigaku MicroMax-007HF'
_exptl_absorpt_coefficient_mu    1.089
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50120
_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_colour            blue
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             5728
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.194
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     767
_refine_ls_number_reflns         53516
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.1168
_refine_ls_R_factor_gt           0.0714
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1248P)^2^+1.3756P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2040
_refine_ls_wR_factor_ref         0.2240
_reflns_number_gt                34105
_reflns_number_total             53516
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00631a2.cif
_cod_data_source_block           compound1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_sg_symbol_H-M      'P n n n'
_cod_database_code               7240497
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              84874
_shelx_fab_checksum              29122