#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:37:03 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179069 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/31/4303146.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4303146
loop_
_publ_author_name
'Chen-Chuan Tsai'
'Tzuoo-Tsair Luo'
'Jen-Fu Yin'
'Hong-Cheu Lin'
'Kuang-Lieh Lu'
_publ_section_title
;
An Unprecedentedly Huge Square-Grid Copper(II)-Organic Framework Material
Built from a Bulky Pyrene-Derived Elongated Cross-Shaped Scaffold
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8650
_journal_page_last               8652
_journal_paper_doi               10.1021/ic900786b
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C40 H38 Cu N4 O7'
_chemical_formula_sum            'C40 H38 Cu N4 O7'
_chemical_formula_weight         750.28
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 124.662(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.2138(11)
_cell_length_b                   35.418(3)
_cell_length_c                   11.9728(10)
_cell_measurement_reflns_used    5323
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      2.84
_cell_volume                     6004.0(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'HKL Denzo and Scalepack'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1027
_diffrn_reflns_av_sigmaI/netI    0.1382
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            22147
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.15
_exptl_absorpt_coefficient_mu    0.398
_exptl_absorpt_correction_T_max  0.9882
_exptl_absorpt_correction_T_min  0.9037
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    0.830
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1564
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         5162
_refine_ls_number_restraints     77
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1221
_refine_ls_R_factor_gt           0.0634
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0928P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1724
_refine_ls_wR_factor_ref         0.1865
_reflns_number_gt                2603
_reflns_number_total             5162
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic900786b_si_002.cif
_cod_data_source_block           sqz_a7557
_cod_original_cell_volume        6004.0(8)
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4303146
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.08612(6) 0.0000 0.61326(10) 0.0474(4) Uani 1 2 d S . .
C1 C -0.0516(5) -0.04937(13) 0.5917(8) 0.0610(18) Uani 1 1 d . . .
C2 C -0.0817(4) -0.07920(13) 0.6514(7) 0.0615(16) Uani 1 1 d . . .
C3 C -0.0137(4) -0.09864(18) 0.7679(8) 0.099(2) Uani 1 1 d . . .
H3 H 0.0501 -0.0932 0.8110 0.119 Uiso 1 1 calc R . .
C4 C -0.0426(4) -0.12606(16) 0.8180(7) 0.100(3) Uani 1 1 d . . .
H4 H 0.0033 -0.1399 0.8929 0.120 Uiso 1 1 calc R . .
C5 C -0.1355(4) -0.13398(12) 0.7634(6) 0.0520(15) Uani 1 1 d . . .
C6 C -0.2018(4) -0.11376(15) 0.6509(6) 0.0716(18) Uani 1 1 d . . .
H6 H -0.2656 -0.1181 0.6114 0.086 Uiso 1 1 calc R . .
C7 C -0.1740(4) -0.08668(14) 0.5952(7) 0.0774(19) Uani 1 1 d . . .
H7 H -0.2199 -0.0735 0.5180 0.093 Uiso 1 1 calc R . .
C8 C -0.1637(4) -0.16275(12) 0.8218(6) 0.0483(14) Uani 1 1 d . . .
C9 C -0.2491(3) -0.19699(11) 0.8609(5) 0.0425(13) Uani 1 1 d . . .
C10 C -0.1575(3) -0.20844(11) 0.9465(5) 0.0397(12) Uani 1 1 d . . .
C11 C -0.1287(3) -0.23849(11) 1.0413(5) 0.0406(13) Uani 1 1 d . . .
C12 C -0.2980(3) -0.24391(11) 0.9561(5) 0.0394(13) Uani 1 1 d . . .
C13 C -0.3241(3) -0.21422(12) 0.8622(5) 0.0448(13) Uani 1 1 d . . .
C14 C -0.4173(4) -0.20235(13) 0.7800(6) 0.0632(17) Uani 1 1 d . A .
H14 H -0.4326 -0.1824 0.7204 0.076 Uiso 1 1 calc R . .
C15 C -0.4891(3) -0.21939(14) 0.7836(6) 0.0649(17) Uani 1 1 d D . .
C16 C -0.4632(4) -0.24860(13) 0.8732(6) 0.0561(16) Uani 1 1 d D . .
C17 C -0.5909(4) -0.2042(2) 0.6908(9) 0.094(5) Uani 0.859(18) 1 d PDU A 1
C18 C -0.6592(6) -0.2250(3) 0.7142(13) 0.118(4) Uani 0.859(18) 1 d PDU A 1
C19 C -0.5912(6) -0.1614(2) 0.7191(13) 0.135(5) Uani 0.859(18) 1 d PDU A 1
C20 C -0.6244(7) -0.2091(4) 0.5409(10) 0.141(5) Uani 0.859(18) 1 d PDU A 1
C17A C -0.5911(11) -0.2057(9) 0.697(3) 0.19(7) Uani 0.141(18) 1 d PDU A 2
C18A C -0.658(3) -0.2394(9) 0.657(4) 0.051(14) Uani 0.141(18) 1 d PDU A 2
C19A C -0.593(3) -0.1795(13) 0.796(5) 0.09(2) Uani 0.141(18) 1 d PDU A 2
C20A C -0.617(4) -0.1833(13) 0.571(4) 0.080(18) Uani 0.141(18) 1 d PDU A 2
O1 O 0.0337(3) -0.03889(9) 0.6665(4) 0.0679(12) Uani 1 1 d . . .
O2 O -0.1135(3) -0.03783(9) 0.4770(5) 0.0665(12) Uani 1 1 d . . .
O3 O 0.2232(5) 0.0000 0.7936(7) 0.127(3) Uani 1 2 d SD . .
O4 O -0.4099(3) -0.11842(13) 0.6318(6) 0.142(2) Uani 1 1 d D . .
N1 N -0.1035(2) -0.18630(9) 0.9198(4) 0.0408(11) Uani 1 1 d . . .
H1 H -0.0435 -0.1876 0.9587 0.049 Uiso 0.50 1 calc PR . .
N2 N -0.2533(2) -0.16773(9) 0.7828(4) 0.0467(11) Uani 1 1 d D . .
H2 H -0.3025 -0.1553 0.7221 0.056 Uiso 0.50 1 calc PR . .
H16 H -0.511(2) -0.2603(10) 0.870(5) 0.056 Uiso 1 1 d D . .
H3A H 0.2817(19) 0.0000 0.835(10) 0.197 Uiso 1 2 d SD . .
H3B H 0.216(7) 0.0000 0.856(8) 0.197 Uiso 1 2 d SD . .
H4A H -0.4108 -0.0953 0.6214 0.224 Uiso 0.50 1 d PD B 1
H4B H -0.4686 -0.1252 0.5936 0.224 Uiso 0.50 1 d PD C 1
H4C H -0.3649 -0.1285 0.7307 0.224 Uiso 0.25 1 d PD D 2
H4D H -0.4108 -0.0953 0.6213 0.224 Uiso 0.25 1 d PD E 2
H4E H -0.3649 -0.1285 0.7307 0.224 Uiso 0.25 1 d PD F 3
H4F H -0.4686 -0.1252 0.5936 0.224 Uiso 0.25 1 d PD G 3
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cu1 O2 87.4(2) 2_556 5_556 ?
O2 Cu1 O1 89.90(15) 2_556 . ?
O2 Cu1 O1 167.95(18) 5_556 . ?
O2 Cu1 O1 167.95(18) 2_556 6 ?
O2 Cu1 O1 89.90(15) 5_556 6 ?
O1 Cu1 O1 90.4(2) . 6 ?
O2 Cu1 O3 94.90(19) 2_556 . ?
O2 Cu1 O3 94.90(19) 5_556 . ?
O1 Cu1 O3 97.03(19) . . ?
O1 Cu1 O3 97.03(19) 6 . ?
O2 Cu1 Cu1 85.10(13) 2_556 5_556 ?
O2 Cu1 Cu1 85.10(13) 5_556 5_556 ?
O1 Cu1 Cu1 82.97(13) . 5_556 ?
O1 Cu1 Cu1 82.97(13) 6 5_556 ?
O3 Cu1 Cu1 180.0(2) . 5_556 ?
O2 C1 O1 127.6(5) . . ?
O2 C1 C2 116.3(6) . . ?
O1 C1 C2 116.1(6) . . ?
C7 C2 C3 118.9(5) . . ?
C7 C2 C1 121.3(6) . . ?
C3 C2 C1 119.8(5) . . ?
C4 C3 C2 118.7(5) . . ?
C5 C4 C3 123.4(6) . . ?
C4 C5 C6 117.1(4) . . ?
C4 C5 C8 121.9(5) . . ?
C6 C5 C8 121.0(5) . . ?
C5 C6 C7 120.5(5) . . ?
C2 C7 C6 121.3(6) . . ?
N1 C8 N2 112.8(4) . . ?
N1 C8 C5 123.7(4) . . ?
N2 C8 C5 123.4(5) . . ?
C10 C9 N2 109.2(3) . . ?
C10 C9 C13 121.8(4) . . ?
N2 C9 C13 129.0(4) . . ?
C9 C10 N1 107.3(4) . . ?
C9 C10 C11 123.4(4) . . ?
N1 C10 C11 129.2(4) . . ?
C16 C11 C12 119.5(4) 7_447 7_447 ?
C16 C11 C10 124.7(4) 7_447 . ?
C12 C11 C10 115.7(4) 7_447 . ?
C13 C12 C11 117.3(4) . 7_447 ?
C13 C12 C12 121.3(4) . 7_447 ?
C11 C12 C12 121.3(5) 7_447 7_447 ?
C14 C13 C12 120.4(4) . . ?
C14 C13 C9 123.2(4) . . ?
C12 C13 C9 116.3(4) . . ?
C13 C14 C15 122.2(4) . . ?
C16 C15 C14 116.8(4) . . ?
C16 C15 C17A 120.7(13) . . ?
C14 C15 C17A 122.5(13) . . ?
C16 C15 C17 123.9(4) . . ?
C14 C15 C17 119.3(5) . . ?
C17A C15 C17 3.3(13) . . ?
C15 C16 C11 123.7(4) . 7_447 ?
C18 C17 C15 112.0(6) . . ?
C18 C17 C20 109.7(7) . . ?
C15 C17 C20 108.5(7) . . ?
C18 C17 C19 109.2(6) . . ?
C15 C17 C19 109.0(6) . . ?
C20 C17 C19 108.4(7) . . ?
C15 C17A C19A 101(3) . . ?
C15 C17A C20A 115(3) . . ?
C19A C17A C20A 109.1(15) . . ?
C15 C17A C18A 109(2) . . ?
C19A C17A C18A 111.7(15) . . ?
C20A C17A C18A 110.6(15) . . ?
C1 O1 Cu1 123.0(4) . . ?
C1 O2 Cu1 121.2(4) . 5_556 ?
C8 N1 C10 105.7(4) . . ?
C8 N2 C9 104.9(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O2 1.940(3) 2_556 ?
Cu1 O2 1.940(3) 5_556 ?
Cu1 O1 1.942(3) . ?
Cu1 O1 1.942(3) 6 ?
Cu1 O3 2.106(7) . ?
Cu1 Cu1 2.6456(19) 5_556 ?
C1 O2 1.235(7) . ?
C1 O1 1.265(6) . ?
C1 C2 1.523(6) . ?
C2 C7 1.353(6) . ?
C2 C3 1.390(7) . ?
C3 C4 1.375(7) . ?
C4 C5 1.368(6) . ?
C5 C6 1.371(7) . ?
C5 C8 1.466(6) . ?
C6 C7 1.398(6) . ?
C8 N1 1.328(5) . ?
C8 N2 1.346(5) . ?
C9 C10 1.364(6) . ?
C9 N2 1.369(5) . ?
C9 C13 1.438(5) . ?
C10 N1 1.385(5) . ?
C10 C11 1.423(6) . ?
C11 C16 1.385(6) 7_447 ?
C11 C12 1.423(5) 7_447 ?
C12 C13 1.413(6) . ?
C12 C11 1.423(5) 7_447 ?
C12 C12 1.432(8) 7_447 ?
C13 C14 1.387(6) . ?
C14 C15 1.398(6) . ?
C15 C16 1.369(6) . ?
C15 C17A 1.523(11) . ?
C15 C17 1.542(7) . ?
C16 C11 1.385(6) 7_447 ?
C17 C18 1.541(7) . ?
C17 C20 1.551(8) . ?
C17 C19 1.555(8) . ?
C17A C19A 1.527(11) . ?
C17A C20A 1.528(11) . ?
C17A C18A 1.530(11) . ?
O2 Cu1 1.940(3) 5_556 ?
