#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:00:57 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178764 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/18/4101826.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_4101826
loop_
_publ_author_name
'Omar K. Farha'
'Christos D. Malliakas'
'Mercouri G. Kanatzidis'
'Joseph T. Hupp'
_publ_contact_author             'Joseph T. Hupp'
_publ_contact_author_email       j-hupp@northwestern.edu
_publ_section_title
;
 Control over Catenation in Metal-Organic Frameworks via Rational Design
 of the Organic Building Block
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              950
_journal_page_last               952
_journal_paper_doi               10.1021/ja909519e
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C22 H12 Br N2 O4 Zn'
_chemical_formula_sum            'C22 H12 Br N2 O4 Zn'
_chemical_formula_weight         513.62
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           10
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2y'
_symmetry_space_group_name_H-M   'P 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                 90.205(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.7110(16)
_cell_length_b                   15.6181(12)
_cell_length_c                   16.0362(19)
_cell_measurement_reflns_used    11889
_cell_measurement_temperature    100(2)
_cell_volume                     2933.1(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1135
_diffrn_reflns_av_sigmaI/netI    0.1295
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15248
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         1.82
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    1.111
_exptl_absorpt_correction_T_max  0.9306
_exptl_absorpt_correction_T_min  0.5089
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   X-Shape2
_exptl_crystal_density_diffrn    0.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             510
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
;
_refine_diff_density_max         3.600
_refine_diff_density_min         -0.995
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.874
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         7645
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      0.877
_refine_ls_R_factor_all          0.1300
_refine_ls_R_factor_gt           0.0956
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1465P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2285
_refine_ls_wR_factor_ref         0.2456
_reflns_number_gt                3857
_reflns_number_total             7645
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja909519e_si_005.cif
_cod_data_source_block           14
_cod_original_sg_symbol_H-M      'P 2/m'
_cod_database_code               4101826
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'-x, -y, -z'
'x, -y, 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
Zn1 Zn 0.50004(6) 0.5000 0.40815(4) 0.03082(19) Uani 1 2 d S . .
Br1 Br 0.72075(7) 0.0000 0.49978(10) 0.1028(5) Uani 1 2 d S . .
O1 O 0.6177(3) 0.4087(2) 0.5700(2) 0.0503(8) Uani 1 1 d . . .
O2 O 0.6195(3) 0.4097(2) 0.4299(2) 0.0503(8) Uani 1 1 d . . .
N1 N 0.4998(5) 0.5000 0.2831(4) 0.0501(14) Uani 1 2 d SD . .
N2 N 0.4533(6) 0.5000 0.0179(6) 0.160(6) Uani 1 2 d SD . .
C1 C 0.8966(4) 0.0000 0.4967(5) 0.0428(16) Uani 1 2 d S . .
C2 C 0.7351(4) 0.3070(3) 0.4993(3) 0.0460(11) Uani 1 1 d . . .
C3 C 0.9386(4) 0.0787(3) 0.4994(3) 0.0431(10) Uani 1 1 d . . .
C4 C 0.8383(5) 0.1976(3) 0.5737(4) 0.0619(15) Uani 1 1 d . . .
H4 H 0.8591 0.1722 0.6240 0.074 Uiso 1 1 calc R . .
C5 C 0.7721(5) 0.2711(3) 0.4261(4) 0.0570(13) Uani 1 1 d . . .
H5 H 0.7516 0.2964 0.3758 0.068 Uiso 1 1 calc R . .
C6 C 0.7720(5) 0.2711(3) 0.5752(3) 0.0588(14) Uani 1 1 d . . .
H6 H 0.7522 0.2963 0.6256 0.071 Uiso 1 1 calc R . .
C7 C 0.8742(4) 0.1609(3) 0.4999(4) 0.0504(12) Uani 1 1 d . . .
C8 C 0.6541(4) 0.3817(2) 0.4993(3) 0.0445(11) Uani 1 1 d . . .
C9 C 0.8398(5) 0.1971(3) 0.4254(4) 0.0618(14) Uani 1 1 d . . .
H9 H 0.8614 0.1726 0.3750 0.074 Uiso 1 1 calc R . .
C10 C 0.3998(8) 0.5000 0.2437(5) 0.137(6) Uani 1 2 d SD . .
H10 H 0.3348 0.5000 0.2768 0.165 Uiso 1 2 calc SR . .
C11 C 0.5899(9) 0.5000 0.2320(6) 0.158(8) Uani 1 2 d SD . .
H11 H 0.6625 0.5000 0.2557 0.190 Uiso 1 2 calc SR . .
C12 C 0.5812(10) 0.5000 0.1440(6) 0.194(10) Uani 1 2 d SD . .
H12 H 0.6469 0.5000 0.1116 0.233 Uiso 1 2 calc SR . .
C13 C 0.4753(11) 0.5000 0.1063(7) 0.170(10) Uani 1 2 d SD . .
C14 C 0.3832(11) 0.5000 0.1606(5) 0.239(15) Uani 1 2 d SD . .
H14 H 0.3092 0.5000 0.1394 0.287 Uiso 1 2 calc SR . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
N N 0.0061 0.0033 '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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
N1 Zn1 O1 100.11(16) . 2_656 ?
N1 Zn1 O1 100.11(16) . 3_666 ?
O1 Zn1 O1 90.1(2) 2_656 3_666 ?
N1 Zn1 O2 99.88(16) . . ?
O1 Zn1 O2 87.13(15) 2_656 . ?
O1 Zn1 O2 160.00(14) 3_666 . ?
N1 Zn1 O2 99.88(16) . 4_565 ?
O1 Zn1 O2 159.99(14) 2_656 4_565 ?
O1 Zn1 O2 87.13(15) 3_666 4_565 ?
O2 Zn1 O2 88.7(2) . 4_565 ?
N1 Zn1 Zn1 179.91(18) . 3_666 ?
O1 Zn1 Zn1 79.82(10) 2_656 3_666 ?
O1 Zn1 Zn1 79.82(10) 3_666 3_666 ?
O2 Zn1 Zn1 80.18(10) . 3_666 ?
O2 Zn1 Zn1 80.18(10) 4_565 3_666 ?
C8 O1 Zn1 128.0(3) . 3_666 ?
C8 O2 Zn1 128.0(3) . . ?
C10 N1 C11 113.8(8) . . ?
C10 N1 Zn1 118.3(6) . . ?
C11 N1 Zn1 127.9(6) . . ?
N2 N2 C13 107.5(12) 2_655 . ?
C3 C1 C3 136.3(5) . 4 ?
C3 C1 Br1 111.7(3) . . ?
C3 C1 Br1 111.7(3) 4 . ?
C5 C2 C6 118.6(4) . . ?
C5 C2 C8 121.2(4) . . ?
C6 C2 C8 120.1(5) . . ?
C1 C3 C3 111.8(3) . 2_756 ?
C1 C3 C7 127.8(4) . . ?
C3 C3 C7 120.4(3) 2_756 . ?
C7 C4 C6 122.0(5) . . ?
C2 C5 C9 121.7(5) . . ?
C4 C6 C2 119.1(5) . . ?
C9 C7 C4 118.8(5) . . ?
C9 C7 C3 119.6(5) . . ?
C4 C7 C3 121.2(5) . . ?
O2 C8 O1 123.9(4) . . ?
O2 C8 C2 118.0(5) . . ?
O1 C8 C2 117.8(4) . . ?
C7 C9 C5 119.6(5) . . ?
N1 C10 C14 126.6(10) . . ?
N1 C11 C12 123.9(10) . . ?
C13 C12 C11 119.9(11) . . ?
C12 C13 C14 115.2(10) . . ?
C12 C13 N2 126.1(10) . . ?
C14 C13 N2 118.8(8) . . ?
C10 C14 C13 120.7(11) . . ?
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
Zn1 N1 2.005(6) . ?
Zn1 O1 2.015(3) 2_656 ?
Zn1 O1 2.015(3) 3_666 ?
Zn1 O2 2.016(3) . ?
Zn1 O2 2.016(3) 4_565 ?
Zn1 Zn1 2.9459(14) 3_666 ?
Br1 C1 2.061(5) . ?
O1 C8 1.284(6) . ?
O1 Zn1 2.015(3) 3_666 ?
O2 C8 1.261(5) . ?
N1 C10 1.329(8) . ?
N1 C11 1.339(8) . ?
N2 N2 1.236(10) 2_655 ?
N2 C13 1.440(8) . ?
C1 C3 1.325(4) . ?
C1 C3 1.325(4) 4 ?
C2 C5 1.372(8) . ?
C2 C6 1.406(7) . ?
C2 C8 1.503(6) . ?
C3 C3 1.438(9) 2_756 ?
C3 C7 1.487(6) . ?
C4 C7 1.383(8) . ?
C4 C6 1.386(7) . ?
C5 C9 1.401(7) . ?
C7 C9 1.382(7) . ?
C10 C14 1.345(8) . ?
C11 C12 1.415(9) . ?
C12 C13 1.378(9) . ?
C13 C14 1.389(9) . ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.025 -0.006 -0.002 2215 685 ' '
