#------------------------------------------------------------------------------
#$Date: 2016-03-21 01:21:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178377 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/17/4001790.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_4001790
loop_
_publ_author_name
'Brozek, Carl K.'
'Cozzolino, Anthony F.'
'Teat, Simon J.'
'Chen, Yu-Sheng'
'Dincă, Mircea'
_publ_section_title
;
 Quantification of Site-Specific Cation Exchange in Metal--Organic
 Frameworks Using Multi-Wavelength Anomalous X-ray Dispersion
;
_journal_issue                   15
_journal_name_full               'Chemistry of Materials'
_journal_page_first              2998
_journal_paper_doi               10.1021/cm400858d
_journal_volume                  25
_journal_year                    2013
_chemical_formula_sum            'C41 H12 Cl Mn7 N48 O5 Zn'
_chemical_formula_weight         1742.39
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           221
_symmetry_space_group_name_Hall  '-P 4 2 3'
_symmetry_space_group_name_H-M   'P m -3 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            4
_cell_length_a                   18.8285(4)
_cell_length_b                   18.8285(4)
_cell_length_c                   18.8285(4)
_cell_measurement_temperature    296(2)
_cell_volume                     6674.9(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0904
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            53913
_diffrn_reflns_theta_full        29.55
_diffrn_reflns_theta_max         29.55
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    1.753
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3424
_refine_diff_density_max         6.296
_refine_diff_density_min         -1.026
_refine_diff_density_rms         0.392
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   4.488
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     54
_refine_ls_number_reflns         1897
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      4.488
_refine_ls_R_factor_all          0.2086
_refine_ls_R_factor_gt           0.1991
_refine_ls_shift/su_max          0.228
_refine_ls_shift/su_mean         0.021
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4940
_refine_ls_wR_factor_ref         0.5026
_reflns_number_gt                1622
_reflns_number_total             1897
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm400858d_si_005.cif
_cod_data_source_block           znmnbtt_16kev_0m
_cod_database_code               4001790
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'
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
Zn1 Zn 0.0000 0.359(3) 0.5000 0.0438(16) Uani 0.75 4 d SP
Mn1 Mn 0.0000 0.358(14) 0.5000 0.0438(16) Uani 0.25 4 d SP
Cl2 Cl 0.0000 0.5000 0.5000 0.0358(12) Uani 1 16 d S
O1 O 0.0000 0.2484(9) 0.5000 0.114(7) Uani 1 4 d S
N1 N 0.0788(3) 0.3702(3) 0.4188(3) 0.0392(12) Uani 1 1 d .
N2 N 0.1339(2) 0.3263(3) 0.4089(3) 0.0399(12) Uani 1 1 d .
C1 C 0.1666(5) 0.3511(3) 0.3511(3) 0.0421(18) Uani 1 2 d S
C2 C 0.2302(4) 0.3206(3) 0.3206(3) 0.0433(18) Uani 1 2 d S
C3 C 0.2605(4) 0.3500(5) 0.2605(4) 0.046(2) Uani 1 2 d S
H3 H 0.2401 0.3901 0.2401 0.056 Uiso 1 2 calc SR
Zn3 Zn 0.1272(2) 0.2624(2) 0.5000 -0.0153(8) Uani 0.06 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'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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'
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
O1 Zn1 N1 95.5(17) . .
O1 Zn1 N1 95.5(17) . 26_556
N1 Zn1 N1 91.2(4) . 26_556
O1 Zn1 N1 95.5(17) . 28
N1 Zn1 N1 87.7(4) . 28
N1 Zn1 N1 169(3) 26_556 28
O1 Zn1 N1 95.5(17) . 3_556
N1 Zn1 N1 169(3) . 3_556
N1 Zn1 N1 87.7(4) 26_556 3_556
N1 Zn1 N1 91.2(4) 28 3_556
O1 Zn1 Cl2 180.000(1) . .
N1 Zn1 Cl2 84.5(17) . .
N1 Zn1 Cl2 84.5(17) 26_556 .
N1 Zn1 Cl2 84.5(17) 28 .
N1 Zn1 Cl2 84.5(17) 3_556 .
O1 Zn1 Zn3 52.7(10) . .
N1 Zn1 Zn3 60.4(7) . .
N1 Zn1 Zn3 60.4(7) 26_556 .
N1 Zn1 Zn3 127.5(16) 28 .
N1 Zn1 Zn3 127.5(16) 3_556 .
Cl2 Zn1 Zn3 127.3(10) . .
O1 Zn1 Zn3 52.7(10) . 3_556
N1 Zn1 Zn3 127.5(16) . 3_556
N1 Zn1 Zn3 127.5(16) 26_556 3_556
N1 Zn1 Zn3 60.4(7) 28 3_556
N1 Zn1 Zn3 60.4(7) 3_556 3_556
Cl2 Zn1 Zn3 127.3(10) . 3_556
Zn3 Zn1 Zn3 105(2) . 3_556
O1 Mn1 N1 96(7) . .
O1 Mn1 N1 96(7) . 26_556
N1 Mn1 N1 91.0(16) . 26_556
O1 Mn1 N1 96(7) . 28
N1 Mn1 N1 87.6(15) . 28
N1 Mn1 N1 167(10) 26_556 28
O1 Mn1 N1 96(7) . 3_556
N1 Mn1 N1 167(10) . 3_556
N1 Mn1 N1 87.6(15) 26_556 3_556
N1 Mn1 N1 91.0(16) 28 3_556
O1 Mn1 Cl2 180.000(1) . .
N1 Mn1 Cl2 84(7) . .
N1 Mn1 Cl2 84(7) 26_556 .
N1 Mn1 Cl2 84(7) 28 .
N1 Mn1 Cl2 84(7) 3_556 .
O1 Mn1 Zn3 53(4) . .
N1 Mn1 Zn3 61(3) . .
N1 Mn1 Zn3 61(3) 26_556 .
N1 Mn1 Zn3 128(6) 28 .
N1 Mn1 Zn3 128(6) 3_556 .
Cl2 Mn1 Zn3 127(4) . .
O1 Mn1 Zn3 53(4) . 3_556
N1 Mn1 Zn3 128(6) . 3_556
N1 Mn1 Zn3 128(6) 26_556 3_556
N1 Mn1 Zn3 61(3) 28 3_556
N1 Mn1 Zn3 61(3) 3_556 3_556
Cl2 Mn1 Zn3 127(4) . 3_556
Zn3 Mn1 Zn3 106(8) . 3_556
Mn1 Cl2 Mn1 180.00(2) 41_565 17_556
Mn1 Cl2 Mn1 90.0 41_565 25_566
Mn1 Cl2 Mn1 90.000(17) 17_556 25_566
Mn1 Cl2 Zn1 90.000(13) 41_565 25_566
Mn1 Cl2 Zn1 90.000(6) 17_556 25_566
Mn1 Cl2 Zn1 0.00(2) 25_566 25_566
Mn1 Cl2 Zn1 180.00(3) 41_565 17_556
Mn1 Cl2 Zn1 0.00(3) 17_556 17_556
Mn1 Cl2 Zn1 90.000(4) 25_566 17_556
Zn1 Cl2 Zn1 90.000(2) 25_566 17_556
Mn1 Cl2 Zn1 0.000(18) 41_565 41_565
Mn1 Cl2 Zn1 180.000(13) 17_556 41_565
Mn1 Cl2 Zn1 90.000(6) 25_566 41_565
Zn1 Cl2 Zn1 90.000(2) 25_566 41_565
Zn1 Cl2 Zn1 180.000(4) 17_556 41_565
Mn1 Cl2 Zn1 90.000(8) 41_565 .
Mn1 Cl2 Zn1 90.000(11) 17_556 .
Mn1 Cl2 Zn1 180.00(3) 25_566 .
Zn1 Cl2 Zn1 180.000(4) 25_566 .
Zn1 Cl2 Zn1 90.0 17_556 .
Zn1 Cl2 Zn1 90.000(5) 41_565 .
Mn1 Cl2 Mn1 90.00(2) 41_565 .
Mn1 Cl2 Mn1 90.0 17_556 .
Mn1 Cl2 Mn1 180.000(16) 25_566 .
Zn1 Cl2 Mn1 180.00(4) 25_566 .
Zn1 Cl2 Mn1 90.000(11) 17_556 .
Zn1 Cl2 Mn1 90.000(8) 41_565 .
Zn1 Cl2 Mn1 0.000(4) . .
Mn1 O1 Zn1 0.00(2) . .
Mn1 O1 Zn3 83.7(4) . .
Zn1 O1 Zn3 83.7(4) . .
Mn1 O1 Zn3 83.7(4) . 3_556
Zn1 O1 Zn3 83.7(4) . 3_556
Zn3 O1 Zn3 167.4(8) . 3_556
N1 N1 N2 109.7(3) 43 .
N1 N1 Zn1 124.9(14) 43 .
N2 N1 Zn1 125.3(15) . .
N1 N1 Mn1 126(6) 43 .
N2 N1 Mn1 125(6) . .
Zn1 N1 Mn1 1(9) . .
N1 N2 C1 104.8(5) . .
N1 N2 Zn3 101.1(4) . .
C1 N2 Zn3 153.5(5) . .
N2 C1 N2 111.0(7) . 43
N2 C1 C2 124.5(4) . .
N2 C1 C2 124.5(4) 43 .
C3 C2 C3 119.0(9) 5 .
C3 C2 C1 120.5(4) 5 .
C3 C2 C1 120.5(4) . .
C2 C3 C2 121.0(9) . 9
C2 C3 H3 119.5 . .
C2 C3 H3 119.5 9 .
N2 Zn3 N2 109.6(4) 26_556 .
N2 Zn3 O1 97.0(3) 26_556 .
N2 Zn3 O1 97.0(3) . .
N2 Zn3 Zn1 72.6(5) 26_556 .
N2 Zn3 Zn1 72.6(5) . .
O1 Zn3 Zn1 43.6(11) . .
N2 Zn3 Mn1 73(2) 26_556 .
N2 Zn3 Mn1 73(2) . .
O1 Zn3 Mn1 43(4) . .
Zn1 Zn3 Mn1 1(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O1 2.09(7) .
Zn1 N1 2.140(8) .
Zn1 N1 2.140(8) 26_556
Zn1 N1 2.140(8) 28
Zn1 N1 2.140(8) 3_556
Zn1 Cl2 2.65(6) .
Zn1 Zn3 3.01(4) .
Zn1 Zn3 3.01(4) 3_556
Mn1 O1 2.1(3) .
Mn1 N1 2.14(3) .
Mn1 N1 2.14(3) 26_556
Mn1 N1 2.14(3) 28
Mn1 N1 2.14(3) 3_556
Mn1 Cl2 2.7(3) .
Mn1 Zn3 2.99(16) .
Mn1 Zn3 2.99(16) 3_556
Cl2 Mn1 2.7(3) 41_565
Cl2 Mn1 2.7(3) 17_556
Cl2 Mn1 2.7(3) 25_566
Cl2 Zn1 2.65(6) 25_566
Cl2 Zn1 2.65(6) 17_556
Cl2 Zn1 2.65(6) 41_565
O1 Zn3 2.410(5) .
O1 Zn3 2.410(5) 3_556
N1 N1 1.295(10) 43
N1 N2 1.340(7) .
N2 C1 1.334(7) .
N2 Zn3 2.100(5) .
C1 N2 1.334(7) 43
C1 C2 1.447(11) .
C2 C3 1.383(6) 5
C2 C3 1.383(6) .
C3 C2 1.383(6) 9
C3 H3 0.9300 .
Zn3 N2 2.100(5) 26_556
