#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:53:39 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179602 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/66/4506608.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_4506608
loop_
_publ_author_name
'Adarsh, N. N.'
'Grélard, Axelle'
'Dufourc, Erick J.'
'Dastidar, Parthasarathi'
_publ_section_title
;
 Sequestering Hydrated Fluoride in a Three-Dimensional
 Non-Interpenetrated Octahedral Coordination Polymer via a
 Single-Crystal-to-Single-Crystal Fashion
;
_journal_issue                   7
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              3369
_journal_paper_doi               10.1021/cg300279z
_journal_volume                  12
_journal_year                    2012
_chemical_formula_sum            'C36 H42 Cl2 Cu N8 O11'
_chemical_formula_weight         897.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           100
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4 -2ab'
_symmetry_space_group_name_H-M   'P 4 b m'
_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                90.00
_cell_formula_units_Z            2
_cell_length_a                   21.6145(4)
_cell_length_b                   21.6145(4)
_cell_length_c                   5.16780(10)
_cell_measurement_temperature    298(2)
_cell_volume                     2414.33(8)
_computing_cell_refinement       'Bruker Apex II'
_computing_data_collection       'Bruker Apex II'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Mercury 2.3'
_computing_publication_material  Shelxl-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       'Omega scan'
_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  0.0537
_diffrn_reflns_av_sigmaI/netI    0.0366
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            26521
_diffrn_reflns_theta_full        28.55
_diffrn_reflns_theta_max         28.55
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    0.621
_exptl_absorpt_correction_T_max  0.9637
_exptl_absorpt_correction_T_min  0.8756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             930
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
;
_refine_diff_density_max         1.152
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.180
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         3167
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0715
_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)+(0.1496P)²+0.7205P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2120
_refine_ls_wR_factor_ref         0.2263
_reflns_number_gt                2765
_reflns_number_total             3167
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             4506221
_cod_data_source_file            cg300279z_si_003.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      P4bm
_cod_database_code               4506608
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'-x+1/2, y+1/2, z'
'-y+1/2, -x+1/2, z'
'x+1/2, -y+1/2, z'
'y+1/2, x+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
Cu1 Cu 1.0000 1.0000 -0.2957(2) 0.0189(3) Uani 1 4 d S
Cl1 Cl 1.0000 1.0000 0.2016(7) 0.0211(3) Uani 1 4 d S
Cl2 Cl 0.67464(17) 0.82536(17) 0.0371(14) 0.0702(14) Uani 0.50 2 d SP
N1 N 0.91190(12) 0.96346(12) -0.2997(9) 0.0205(6) Uani 1 1 d .
C2 C 0.87016(17) 0.98429(18) -0.4662(10) 0.0250(8) Uani 1 1 d .
H2 H 0.8812 1.0159 -0.5791 0.030 Uiso 1 1 calc R
C3 C 0.81005(18) 0.96025(19) -0.4780(11) 0.0315(9) Uani 1 1 d .
H3 H 0.7816 0.9753 -0.5974 0.038 Uiso 1 1 calc R
C4 C 0.79407(16) 0.91333(18) -0.3065(12) 0.0315(9) Uani 1 1 d .
H4 H 0.7545 0.8965 -0.3095 0.038 Uiso 1 1 calc R
C5 C 0.83762(17) 0.89176(17) -0.1309(9) 0.0242(8) Uani 1 1 d .
C6 C 0.89613(17) 0.91916(17) -0.1312(9) 0.0218(7) Uani 1 1 d .
H6 H 0.9252 0.9062 -0.0101 0.026 Uiso 1 1 calc R
N7 N 0.81999(16) 0.84374(17) 0.0380(9) 0.0276(7) Uani 1 1 d .
H7 H 0.7810 0.8386 0.0637 0.033 Uiso 1 1 calc R
C8 C 0.85903(18) 0.80482(18) 0.1639(9) 0.0273(9) Uani 1 1 d .
O9 O 0.91541(14) 0.81079(15) 0.1708(10) 0.0452(10) Uani 1 1 d .
C10 C 0.82785(18) 0.75142(18) 0.2941(9) 0.0249(8) Uani 1 1 d .
C11 C 0.77541(18) 0.72459(18) 0.1866(14) 0.0262(11) Uani 1 2 d S
H11 H 0.7579 0.7421 0.0395 0.031 Uiso 1 2 calc SR
C12 C 0.85479(19) 0.7241(2) 0.5092(10) 0.0308(9) Uani 1 1 d .
H12 H 0.8906 0.7409 0.5801 0.037 Uiso 1 1 calc R
C13 C 0.8285(2) 0.6715(2) 0.6196(14) 0.0348(14) Uani 1 2 d S
H13 H 0.8459 0.6541 0.7668 0.042 Uiso 1 2 calc SR
O13 O 0.9782(5) 0.6971(5) 0.034(3) 0.037(3) Uani 0.25 1 d P
O14 O 0.6484(5) 0.9912(5) 0.536(3) 0.026(2) Uiso 0.25 1 d P
O15 O 0.6332(3) 0.8668(3) 0.532(3) 0.055(3) Uani 0.50 2 d SP
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'
H H 0.0000 0.0000 '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
N1 Cu1 N1 89.995(4) 2_755 .
N1 Cu1 N1 89.996(6) 2_755 3_775
N1 Cu1 N1 178.9(3) . 3_775
N1 Cu1 N1 178.9(3) 2_755 4_575
N1 Cu1 N1 89.994(6) . 4_575
N1 Cu1 N1 89.993(4) 3_775 4_575
N1 Cu1 Cl1 90.57(13) 2_755 .
N1 Cu1 Cl1 90.57(13) . .
N1 Cu1 Cl1 90.57(13) 3_775 .
N1 Cu1 Cl1 90.57(13) 4_575 .
N1 Cu1 Cl1 89.43(13) 2_755 1_554
N1 Cu1 Cl1 89.43(13) . 1_554
N1 Cu1 Cl1 89.43(13) 3_775 1_554
N1 Cu1 Cl1 89.43(13) 4_575 1_554
Cl1 Cu1 Cl1 179.999(1) . 1_554
Cu1 Cl1 Cu1 180.0 . 1_556
C2 N1 C6 119.5(3) . .
C2 N1 Cu1 120.3(3) . .
C6 N1 Cu1 120.2(3) . .
N1 C2 C3 122.2(4) . .
C4 C3 C2 118.2(4) . .
C5 C4 C3 119.6(3) . .
C4 C5 C6 118.1(4) . .
C4 C5 N7 118.0(3) . .
C6 C5 N7 123.9(3) . .
N1 C6 C5 122.4(4) . .
C8 N7 C5 125.8(3) . .
O9 C8 N7 124.5(4) . .
O9 C8 C10 121.1(4) . .
N7 C8 C10 114.4(3) . .
C12 C10 C11 119.0(4) . .
C12 C10 C8 120.0(3) . .
C11 C10 C8 120.7(4) . .
C10 C11 C10 121.4(6) . 6_665
C10 C12 C13 120.3(4) . .
C12 C13 C12 119.9(6) 6_665 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N1 2.061(3) 2_755
Cu1 N1 2.062(3) .
Cu1 N1 2.062(3) 3_775
Cu1 N1 2.062(3) 4_575
Cu1 Cl1 2.570(3) .
Cu1 Cl1 2.598(3) 1_554
Cl1 Cu1 2.598(3) 1_556
N1 C2 1.326(5) .
N1 C6 1.338(5) .
C2 C3 1.401(5) .
C3 C4 1.390(6) .
C4 C5 1.388(6) .
C5 C6 1.396(5) .
C5 N7 1.409(5) .
N7 C8 1.358(5) .
C8 O9 1.226(5) .
C8 C10 1.496(5) .
C10 C12 1.387(6) .
C10 C11 1.389(5) .
C11 C10 1.389(5) 6_665
C12 C13 1.393(5) .
C13 C12 1.393(5) 6_665
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
1 0.000 0.500 0.024 140.7 37.5
2 0.500 0.000 0.029 140.7 37.6
