#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/56/4315664.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_4315664
loop_
_publ_author_name
'Choong-Sun Lim'
'Jennifer K. Schnobrich'
'Antek G. Wong-Foy'
'Adam J. Matzger'
_publ_contact_author_address
'Dept. of Chem., University of Michigan, 930 N. University, Ann Arbor, MI 48109'
_publ_contact_author_email       matzger@umich.edu
_publ_contact_author_fax         '(734) 647-4865'
_publ_contact_author_name        'Adam J. Matzger'
_publ_contact_author_phone       '(734) 615-6627'
_publ_section_title
;
 Metal-Dependent Phase Selection in Coordination Polymers Derived from a
 C2v-Symmetric Tricarboxylate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5271
_journal_page_last               5275
_journal_paper_doi               10.1021/ic100378p
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C30 H14 Cu2 Fe1 O15.33'
_chemical_formula_sum            'C30 H14 Cu2 Fe O15.33'
_chemical_formula_weight         802.6503
_chemical_name_common            FeCuBPTC-5
_chemical_name_systematic        FeCuBPTC-5
_space_group_IT_number           194
_symmetry_cell_setting           hexagonal
_symmetry_Int_Tables_number      194
_symmetry_space_group_name_Hall  '-P 6c 2c'
_symmetry_space_group_name_H-M   'P 63/m m c'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   18.452(3)
_cell_length_b                   18.452(3)
_cell_length_c                   40.925(11)
_cell_measurement_reflns_used    6567
_cell_measurement_temperature    253(2)
_cell_measurement_theta_max      50.4
_cell_measurement_theta_min      2.8
_cell_volume                     12067(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      253(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku RAXIS-Rapid'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0714
_diffrn_reflns_av_sigmaI/netI    0.0477
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            24287
_diffrn_reflns_theta_full        50.50
_diffrn_reflns_theta_max         50.50
_diffrn_reflns_theta_min         2.16
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.302
_exptl_absorpt_correction_T_max  0.924
_exptl_absorpt_correction_T_min  0.725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    0.663
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Hexagon
_exptl_crystal_F_000             2404
_exptl_crystal_recrystallization_method 'solvothermal reaction'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.032
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         2414
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0613P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1141
_reflns_number_gt                2013
_reflns_number_total             2414
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100378p_si_002_1.cif
_cod_data_source_block           Compound-5
_cod_original_cell_volume        12067(5)
_cod_original_formula_sum        'C30 H14 Cu2 Fe1 O15.33'
_cod_database_code               4315664
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'-x+y, y, z'
'y, x, z+1/2'
'x, x-y, z'
'x-y, -y, z+1/2'
'-y, -x, z'
'-x, -x+y, z+1/2'
'-x, -y, -z'
'-x+y, -x, -z-1/2'
'y, -x+y, -z'
'x, y, -z-1/2'
'x-y, x, -z'
'-y, x-y, -z-1/2'
'x-y, -y, -z'
'-y, -x, -z-1/2'
'-x, -x+y, -z'
'-x+y, y, -z-1/2'
'y, x, -z'
'x, x-y, -z-1/2'
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 0.523955(16) 0.04791(3) 0.474058(13) 0.0637(3) Uani 1 2 d S . .
Fe1 Fe 1.05846(3) 0.11692(5) 0.7500 0.0620(3) Uani 1 4 d S . .
O1 O 1.13828(14) 0.12909(13) 0.71615(5) 0.1061(8) Uani 1 1 d . . .
O2 O 1.1299(3) 0.2598(5) 0.7500 0.284(4) Uani 1 4 d S . .
O3 O 1.0000 0.0000 0.7500 0.174(4) Uani 1 12 d S . .
O4 O 0.48132(11) 0.10954(11) 0.49825(5) 0.0766(6) Uani 1 1 d . . .
O5 O 0.56093(11) -0.02714(12) 0.45724(5) 0.0761(6) Uani 1 1 d . . .
O6 O 0.56717(12) 0.1343(2) 0.43170(9) 0.200(2) Uani 1 2 d S . .
C1 C 0.6407(2) 0.0902(2) 0.52631(9) 0.0724(9) Uani 1 1 d . . .
C2 C 0.72236(19) 0.14669(18) 0.54192(7) 0.0719(8) Uani 1 1 d . . .
C3 C 0.77679(12) 0.22321(12) 0.52746(9) 0.0713(12) Uani 1 2 d S . .
H1 H 0.7619 0.2381 0.5079 0.086 Uiso 1 2 calc SR . .
C4 C 0.7461(2) 0.12632(18) 0.57141(7) 0.0776(9) Uani 1 1 d . . .
H2 H 0.7093 0.0761 0.5816 0.093 Uiso 1 1 calc R . .
C5 C 0.82204(13) 0.17796(13) 0.58578(11) 0.0792(13) Uani 1 2 d S A .
C6 C 0.84541(16) 0.15459(16) 0.61661(12) 0.0830(14) Uani 1 2 d S . .
C7 C 0.7838(10) 0.0943(10) 0.6377(4) 0.097(4) Uani 0.43(2) 1 d P A 1
H7 H 0.7271 0.0689 0.6326 0.116 Uiso 0.43(2) 1 calc PR A 1
C8 C 0.8116(8) 0.0740(9) 0.6669(4) 0.082(5) Uani 0.43(2) 1 d P A 1
H8 H 0.7714 0.0377 0.6816 0.098 Uiso 0.43(2) 1 calc PR A 1
C71 C 0.8132(9) 0.0741(9) 0.6261(4) 0.124(5) Uani 0.57(2) 1 d P A 2
H71 H 0.7735 0.0334 0.6124 0.149 Uiso 0.57(2) 1 calc PR A 2
C81 C 0.8337(12) 0.0461(9) 0.6545(4) 0.156(7) Uani 0.57(2) 1 d P A 2
H81 H 0.8070 -0.0106 0.6597 0.187 Uiso 0.57(2) 1 calc PR A 2
C9 C 0.89492(15) 0.10508(15) 0.67466(11) 0.0739(12) Uani 1 2 d S . .
C10 C 0.92131(14) 0.07869(14) 0.70452(11) 0.0768(13) Uani 1 2 d S . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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
O4 Cu1 O4 88.29(11) 7_655 . ?
O4 Cu1 O5 169.08(8) 7_655 7_655 ?
O4 Cu1 O5 89.99(8) . 7_655 ?
O4 Cu1 O5 89.99(8) 7_655 . ?
O4 Cu1 O5 169.08(8) . . ?
O5 Cu1 O5 89.66(11) 7_655 . ?
O4 Cu1 O6 94.73(10) 7_655 . ?
O4 Cu1 O6 94.74(10) . . ?
O5 Cu1 O6 96.15(10) 7_655 . ?
O5 Cu1 O6 96.15(10) . . ?
O4 Cu1 Cu1 83.30(6) 7_655 13_656 ?
O4 Cu1 Cu1 83.30(6) . 13_656 ?
O5 Cu1 Cu1 85.79(6) 7_655 13_656 ?
O5 Cu1 Cu1 85.79(6) . 13_656 ?
O6 Cu1 Cu1 177.25(12) . 13_656 ?
O3 Fe1 O1 95.72(7) . 16_557 ?
O3 Fe1 O1 95.72(7) . 22_757 ?
O1 Fe1 O1 88.41(13) 16_557 22_757 ?
O3 Fe1 O1 95.72(7) . . ?
O1 Fe1 O1 90.45(14) 16_557 . ?
O1 Fe1 O1 168.56(13) 22_757 . ?
O3 Fe1 O1 95.72(7) . 7_755 ?
O1 Fe1 O1 168.56(14) 16_557 7_755 ?
O1 Fe1 O1 90.45(14) 22_757 7_755 ?
O1 Fe1 O1 88.41(13) . 7_755 ?
O3 Fe1 O2 180.00(5) . . ?
O1 Fe1 O2 84.28(7) 16_557 . ?
O1 Fe1 O2 84.28(7) 22_757 . ?
O1 Fe1 O2 84.28(7) . . ?
O1 Fe1 O2 84.28(7) 7_755 . ?
C10 O1 Fe1 131.8(3) 5_765 . ?
Fe1 O3 Fe1 120.0 14_767 . ?
Fe1 O3 Fe1 119.999(1) 14_767 3_645 ?
Fe1 O3 Fe1 120.0 . 3_645 ?
C1 O4 Cu1 124.5(2) 7_655 . ?
C1 O5 Cu1 121.0(2) 19_556 . ?
O4 C1 O5 125.3(3) 7_655 19_556 ?
O4 C1 C2 117.4(3) 7_655 . ?
O5 C1 C2 117.2(3) 19_556 . ?
C3 C2 C4 118.4(3) . . ?
C3 C2 C1 119.7(3) . . ?
C4 C2 C1 121.9(3) . . ?
C2 C3 C2 120.6(4) . 11_665 ?
C5 C4 C2 122.1(3) . . ?
C4 C5 C4 118.2(4) . 11_665 ?
C4 C5 C6 120.86(19) . . ?
C4 C5 C6 120.86(19) 11_665 . ?
C71 C6 C71 100.7(13) 11_665 . ?
C71 C6 C7 39.1(6) 11_665 11_665 ?
C71 C6 C7 116.4(5) . 11_665 ?
C71 C6 C7 116.4(5) 11_665 . ?
C71 C6 C7 39.1(6) . . ?
C7 C6 C7 105.0(13) 11_665 . ?
C71 C6 C5 122.5(6) 11_665 . ?
C71 C6 C5 122.5(6) . . ?
C7 C6 C5 121.1(6) 11_665 . ?
C7 C6 C5 121.1(6) . . ?
C6 C7 C8 117.7(11) . . ?
C9 C8 C7 123.8(10) . . ?
C6 C71 C81 126.3(10) . . ?
C9 C81 C71 118.0(10) . . ?
C81 C9 C81 106.8(14) . 11_665 ?
C81 C9 C8 117.4(6) . 11_665 ?
C81 C9 C8 40.1(7) 11_665 11_665 ?
C81 C9 C8 40.1(7) . . ?
C81 C9 C8 117.4(6) 11_665 . ?
C8 C9 C8 99.6(12) 11_665 . ?
C81 C9 C10 120.3(6) . . ?
C81 C9 C10 120.3(6) 11_665 . ?
C8 C9 C10 122.1(6) 11_665 . ?
C8 C9 C10 122.1(6) . . ?
O1 C10 O1 125.8(4) 7_755 3_645 ?
O1 C10 C9 117.1(2) 7_755 . ?
O1 C10 C9 117.1(2) 3_645 . ?
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 O4 1.9459(19) 7_655 ?
Cu1 O4 1.9460(19) . ?
Cu1 O5 1.9500(19) 7_655 ?
Cu1 O5 1.9500(19) . ?
Cu1 O6 2.217(3) . ?
Cu1 Cu1 2.6179(11) 13_656 ?
Fe1 O3 1.8684(9) . ?
Fe1 O1 1.951(2) 16_557 ?
Fe1 O1 1.951(2) 22_757 ?
Fe1 O1 1.951(2) . ?
Fe1 O1 1.951(2) 7_755 ?
Fe1 O2 2.283(9) . ?
O1 C10 1.242(2) 5_765 ?
O3 Fe1 1.8684(9) 14_767 ?
O3 Fe1 1.8685(9) 3_645 ?
O4 C1 1.258(3) 7_655 ?
O5 C1 1.273(4) 19_556 ?
C1 O4 1.258(3) 7_655 ?
C1 O5 1.273(4) 19_556 ?
C1 C2 1.482(4) . ?
C2 C3 1.391(3) . ?
C2 C4 1.398(3) . ?
C3 C2 1.391(3) 11_665 ?
C4 C5 1.371(3) . ?
C5 C4 1.371(3) 11_665 ?
C5 C6 1.466(6) . ?
C6 C71 1.351(13) 11_665 ?
C6 C71 1.351(13) . ?
C6 C7 1.419(15) 11_665 ?
C6 C7 1.419(15) . ?
C7 C8 1.423(18) . ?
C8 C9 1.383(13) . ?
C71 C81 1.402(14) . ?
C81 C9 1.382(13) . ?
C9 C81 1.382(13) 11_665 ?
C9 C8 1.383(13) 11_665 ?
C9 C10 1.485(5) . ?
C10 O1 1.242(2) 7_755 ?
C10 O1 1.242(2) 3_645 ?
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 -0.047 -0.030 -0.001 8321 1689 ' '
