Engineering New Metal-Organic Frameworks Built from Flexible Tetrapyridines Coordinated to Cu(II) and Cu(I)
Patrick E. Ryan; Christophe Lescop; Dominic Laliberté; Tamara Hamilton; Thierry Maris; James D. Wuest; Inorganic Chemistry 48 (2009) 2793–2807; doi:10.1021/ic8019809

data_4301791
_publ_contact_author_address
;
D\'epartement de Chimie, 
Universit\'e de Montr\'eal,
Montr\'eal, Qu\'ebec H3C 3J7, Canada
;
_publ_contact_author_email       james.d.wuest@umontreal.ca
_publ_contact_author_fax         '1 (514) 340-5290'
_publ_contact_author_name        'James D. Wuest'
_publ_contact_author_phone       '1 (514) 340-5178'
_publ_section_title
;
Engineering New Metal-Organic Frameworks Built from Flexible Tetrapyridines
Coordinated to Cu(II) and Cu(I)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2793
_journal_page_last               2807
_journal_paper_doi               10.1021/ic8019809
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety
'C49 H40 N4 O4, Cu (NO3)2, 2(C3 H7 N O), 8(H2 O)'
_chemical_formula_sum            'C55 H70 Cu N8 O20'
_chemical_formula_weight         1226.73
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           50
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2b'
_symmetry_space_group_name_H-M   'P b a n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   39.952(5)
_cell_length_b                   15.031(2)
_cell_length_c                   16.253(2)
_cell_measurement_reflns_used    28753
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      67.169
_cell_measurement_theta_min      2.7175
_cell_volume                     9760(2)
_computing_cell_refinement       'SAINT V6.35A (Bruker AXS, 2002)'
_computing_data_collection       'SMART v5.059 (Bruker, 1999)'
_computing_data_reduction        'SAINT V6.35A (Bruker AXS, 2002)'
_computing_molecular_graphics    'ATOMS (Dowty, 2003)'
_computing_publication_material  'UdMX (Maris, 2004)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker AXS Smart 2k/Platform'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray Sealed Tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0740
_diffrn_reflns_av_sigmaI/netI    0.0975
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            85712
_diffrn_reflns_theta_full        70.10
_diffrn_reflns_theta_max         70.10
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        0.00
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    0.735
_exptl_absorpt_correction_T_max  0.9500
_exptl_absorpt_correction_T_min  0.8233
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs Sheldrick, 2002)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    0.835
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2580
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
Attempts to  model disordered solvent molecules
were unsuccessful. PLATON/SQUEEZE  was used to correct
the data for the presence of the disordered solvent.
A potential solvent volume of 2616.4 \%A^3^, 
26.8 % of the total unit-cell volume, was found.
608 electrons per unit cell worth of scattering were located
in the void. The reported structure is based on the 
PLATON/SQUEEZE corrected data. The actual solvent content is
unknown, so several quantities calculated like empirical formula, density, 
absorption coefficient, F(000) etc. may be incorrect.

Ref:  Sluis, P. van der & Spek, A.L. (1990). Acta Cryst. A46, 194-201.
;
_refine_diff_density_max         0.728
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.164
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.863
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         9235
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      0.943
_refine_ls_R_factor_all          0.1367
_refine_ls_R_factor_gt           0.0645
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.2243
_reflns_number_gt                3458
_reflns_number_total             9235
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic8019809_si_001_5.cif
_cod_data_source_block           jiw452
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P b a n'
_cod_database_code               4301791