Crystallization and structural properties of a family of isotopological 3D-networks: the case of a 4,4′-bipy ligand‒M2+ triflate system
Rizzato, Silvia; Moret, Massimo; Beghi, Fabio; Lo Presti, Leonardo; CrystEngComm 20 (2018) 3784–; doi:10.1039/C8CE00653A

data_7230732
_publ_section_title
;
 Crystallization and structural properties of a family of isotopological
 3D-networks: the case of a 4,4&#x2032;-bipy ligand--M2+ triflate system
;
_journal_issue                   26
_journal_name_full               CrystEngComm
_journal_page_first              3784
_journal_paper_doi               10.1039/C8CE00653A
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety
'(C21.625 H16.75 F4.875 Fe N4 O5.25 S1.625), 0.375(C F3 O3 S)'
_chemical_formula_sum            'C22 H16.75 F6 Fe N4 O6.375 S2'
_chemical_formula_weight         673.11
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      70
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2018-03-29 deposited with the CCDC.
2018-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            32
_cell_length_a                   16.993(9)
_cell_length_b                   42.006(2)
_cell_length_c                   42.426(2)
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      23.96
_cell_measurement_theta_min      2.37
_cell_volume                     30284(16)
_computing_molecular_graphics
'VESTA 3: K. Momma and F. Izumi, J. Appl. Crystallogr.(2011),44,127'
_computing_publication_material
'WinGX: Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838'
_computing_structure_refinement
'SHELX: Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122'
_computing_structure_solution
'SIR 2014: C. Giacovazzo et all., J. Appl. Cryst.(2015) 48, 306'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 CCD_plate
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'bruker smart apex ccd diffractometer'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_av_unetI/netI     0.027
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            62609
_diffrn_reflns_theta_full        23.97
_diffrn_reflns_theta_max         23.97
_diffrn_reflns_theta_min         1.92
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.572
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.6616
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sadabs 2.01 (Bruker AXS, 1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'polyhedral block'
_exptl_crystal_F_000             10872
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;
 Attempts to refine peaks of residual electron density as guest
 atoms were unsuccessful. The data were corrected for disordered
 electron density through use of the SQUEEZE procedure (Sluis, P. van der;
 Spek, A. L. Acta Crystallogr. 1990, A46, 194-201) as implemented in PLATON
 (Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13)
 A total solvent-accessible surface of 3237.24 A^3^ (10,7%) and a 
 contact surface of 8373,03 A^3^ (27.6%)
;
_refine_diff_density_max         1.498
_refine_diff_density_min         -1.174
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.472
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         5899
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.471
_refine_ls_R_factor_all          0.1178
_refine_ls_R_factor_gt           0.1085
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3232
_refine_ls_wR_factor_ref         0.3311
_reflns_number_gt                4978
_reflns_number_total             5899
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8ce00653a2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7230729--7230734.cif.
;
_cod_original_cell_volume        30283(3)
_cod_original_sg_symbol_H-M      Fddd
_cod_database_code               7230732