#------------------------------------------------------------------------------
#$Date: 2016-03-21 01:21:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178377 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/17/4001787.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_4001787
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 Cu Mn7 N48 O5'
_chemical_formula_weight         1740.56
_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            2
_cell_length_a                   18.4852(5)
_cell_length_b                   18.4852(5)
_cell_length_c                   18.4852(5)
_cell_measurement_temperature    296(2)
_cell_volume                     6316.4(3)
_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  0.0468
_diffrn_reflns_av_sigmaI/netI    0.0165
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            45077
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    0.905
_exptl_crystal_density_diffrn    0.915
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1710
_refine_diff_density_max         2.163
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.883
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     54
_refine_ls_number_reflns         1489
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.883
_refine_ls_R_factor_all          0.1441
_refine_ls_R_factor_gt           0.1291
_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)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3587
_refine_ls_wR_factor_ref         0.4042
_reflns_number_gt                1194
_reflns_number_total             1489
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm400858d_si_002.cif
_cod_data_source_block           cumnbtt_16kev_0m
_cod_database_code               4001787
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
Cu1 Cu 0.5000 0.36360(12) 0.0000 0.0565(8) Uani 0.90 4 d SP
Mn1 Mn 0.5000 0.348(2) 0.0000 0.0565(8) Uani 0.10 4 d SP
Cl1 Cl 0.5000 0.5000 0.0000 0.0752(15) Uani 1 16 d S
O1 O 0.5000 0.2395(6) 0.0000 0.134(5) Uani 1 4 d S
N1 N 0.4203(2) 0.3697(2) 0.0750(2) 0.0597(11) Uani 1 1 d .
N2 N 0.4095(2) 0.3247(2) 0.1304(2) 0.0631(11) Uani 1 1 d .
C1 C 0.3508(3) 0.3508(3) 0.1623(4) 0.0625(17) Uani 1 2 d S
C2 C 0.3191(3) 0.3191(3) 0.2276(4) 0.0674(18) Uani 1 2 d S
C3 C 0.3484(4) 0.2577(3) 0.2577(3) 0.0645(17) Uani 1 2 d S
H3 H 0.3885 0.2362 0.2361 0.077 Uiso 1 2 calc SR
Cu2 Cu 0.5000 0.2565(4) 0.1370(4) 0.0246(14) 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'
Cu Cu 0.3201 1.2651 '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 93.2(2) . 28_655
N1 Cu1 N1 86.4(2) . 26
N1 Cu1 N1 173.6(3) 28_655 26
N1 Cu1 N1 173.6(3) . 3_655
N1 Cu1 N1 86.4(2) 28_655 3_655
N1 Cu1 N1 93.2(2) 26 3_655
N1 Cu1 O1 93.20(13) . .
N1 Cu1 O1 93.20(13) 28_655 .
N1 Cu1 O1 93.20(13) 26 .
N1 Cu1 O1 93.20(13) 3_655 .
N1 Cu1 Cl1 86.80(13) . .
N1 Cu1 Cl1 86.80(13) 28_655 .
N1 Cu1 Cl1 86.80(13) 26 .
N1 Cu1 Cl1 86.80(13) 3_655 .
O1 Cu1 Cl1 180.0 . .
N1 Mn1 N1 91.2(5) . 28_655
N1 Mn1 N1 84.6(5) . 26
N1 Mn1 N1 158(2) 28_655 26
N1 Mn1 N1 158(2) . 3_655
N1 Mn1 N1 84.6(5) 28_655 3_655
N1 Mn1 N1 91.2(5) 26 3_655
N1 Mn1 O1 101.1(12) . .
N1 Mn1 O1 101.1(12) 28_655 .
N1 Mn1 O1 101.1(12) 26 .
N1 Mn1 O1 101.1(12) 3_655 .
N1 Mn1 Cl1 78.9(12) . .
N1 Mn1 Cl1 78.9(12) 28_655 .
N1 Mn1 Cl1 78.9(12) 26 .
N1 Mn1 Cl1 78.9(12) 3_655 .
O1 Mn1 Cl1 180.0 . .
Mn1 Cl1 Mn1 180.0 37_665 13
Mn1 Cl1 Mn1 90.000(1) 37_665 25_665
Mn1 Cl1 Mn1 90.000(2) 13 25_665
Mn1 Cl1 Cu1 90.0 37_665 25_665
Mn1 Cl1 Cu1 90.0 13 25_665
Mn1 Cl1 Cu1 0.000(2) 25_665 25_665
Mn1 Cl1 Cu1 180.0 37_665 13
Mn1 Cl1 Cu1 0.0 13 13
Mn1 Cl1 Cu1 90.000(2) 25_665 13
Cu1 Cl1 Cu1 90.0 25_665 13
Mn1 Cl1 Cu1 0.0 37_665 37_665
Mn1 Cl1 Cu1 180.0 13 37_665
Mn1 Cl1 Cu1 90.000(1) 25_665 37_665
Cu1 Cl1 Cu1 90.0 25_665 37_665
Cu1 Cl1 Cu1 180.0 13 37_665
Mn1 Cl1 Cu1 90.000(1) 37_665 .
Mn1 Cl1 Cu1 90.000(1) 13 .
Mn1 Cl1 Cu1 180.000(2) 25_665 .
Cu1 Cl1 Cu1 180.0 25_665 .
Cu1 Cl1 Cu1 90.0 13 .
Cu1 Cl1 Cu1 90.0 37_665 .
Mn1 Cl1 Mn1 90.000(1) 37_665 .
Mn1 Cl1 Mn1 90.000(2) 13 .
Mn1 Cl1 Mn1 180.000(1) 25_665 .
Cu1 Cl1 Mn1 180.000(3) 25_665 .
Cu1 Cl1 Mn1 90.000(2) 13 .
Cu1 Cl1 Mn1 90.000(1) 37_665 .
Cu1 Cl1 Mn1 0.0 . .
Mn1 O1 Cu1 0.000(1) . .
N2 N1 N1 109.6(2) . 38
N2 N1 Mn1 120.2(10) . .
N1 N1 Mn1 129.9(9) 38 .
N2 N1 Cu1 126.8(3) . .
N1 N1 Cu1 123.60(12) 38 .
Mn1 N1 Cu1 7.9(12) . .
N1 N2 C1 103.7(4) . .
N1 N2 Cu2 107.5(3) . .
C1 N2 Cu2 147.7(4) . .
N2 C1 N2 113.4(6) 38 .
N2 C1 C2 123.3(3) 38 .
N2 C1 C2 123.3(3) . .
C3 C2 C3 119.2(7) 5 .
C3 C2 C1 120.4(4) 5 .
C3 C2 C1 120.4(4) . .
C2 C3 C2 120.8(7) . 9
C2 C3 H3 119.6 . .
C2 C3 H3 119.6 9 .
N2 Cu2 N2 105.7(4) . 28_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N1 2.026(4) .
Cu1 N1 2.026(4) 28_655
Cu1 N1 2.026(4) 26
Cu1 N1 2.026(4) 3_655
Cu1 O1 2.294(11) .
Cu1 Cl1 2.521(2) .
Mn1 N1 2.061(9) .
Mn1 N1 2.061(9) 28_655
Mn1 N1 2.061(9) 26
Mn1 N1 2.061(9) 3_655
Mn1 O1 2.01(4) .
Mn1 Cl1 2.80(4) .
Cl1 Mn1 2.80(4) 37_665
Cl1 Mn1 2.80(4) 13
Cl1 Mn1 2.80(4) 25_665
Cl1 Cu1 2.521(2) 25_665
Cl1 Cu1 2.521(2) 13
Cl1 Cu1 2.521(2) 37_665
N1 N2 1.333(5) .
N1 N1 1.323(8) 38
N2 C1 1.326(6) .
N2 Cu2 2.098(6) .
C1 N2 1.326(6) 38
C1 C2 1.465(10) .
C2 C3 1.375(5) 5
C2 C3 1.375(5) .
C3 C2 1.375(5) 9
C3 H3 0.9300 .
Cu2 N2 2.098(6) 28_655
