#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/80/4118052.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_4118052
loop_
_publ_author_name
'Jian Tian'
'Laxmikant V. Saraf'
'Birgit Schwenzer'
'Stephanie M. Taylor'
'Euan K. Brechin'
'Jun Liu'
'Scott J. Dalgarno'
'Praveen K. Thallapally'
_publ_section_title
;
 Selective Metal Cation Capture by Soft Anionic Metal-Organic Frameworks
 via Drastic Single-Crystal-to-Single-Crystal Transformations
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9581
_journal_page_last               9584
_journal_paper_doi               10.1021/ja303092m
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C33 H24 Mn0.5 Ni1.5 O16'
_chemical_formula_weight         792.06
_chemical_name_common            3
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.215(2)
_cell_angle_beta                 98.782(2)
_cell_angle_gamma                114.858(2)
_cell_formula_units_Z            2
_cell_length_a                   16.6187(7)
_cell_length_b                   15.6802(6)
_cell_length_c                   16.8631(7)
_cell_measurement_temperature    100(2)
_cell_volume                     3541.2(3)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'Apex II'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'XSeed (Barbour, 2001)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.885
_diffrn_measured_fraction_theta_max 0.885
_diffrn_measurement_device_type  'Bruker X8 Apex II CCD Diffractometer'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0674
_diffrn_reflns_av_sigmaI/netI    0.1226
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            38542
_diffrn_reflns_theta_full        25.44
_diffrn_reflns_theta_max         25.44
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    0.524
_exptl_absorpt_correction_T_max  0.9255
_exptl_absorpt_correction_T_min  0.8801
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Bruker-SADABS
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    0.743
_exptl_crystal_description       Block
_exptl_crystal_F_000             809
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.479
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         11576
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1299
_refine_ls_R_factor_gt           0.0789
_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)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1994
_refine_ls_wR_factor_ref         0.2168
_reflns_number_gt                5445
_reflns_number_total             11576
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja303092m_si_006.cif
_cod_data_source_block           3
_cod_original_cell_volume        3541.2(2)
_cod_original_formula_sum        'C33 H24 Mn0.50 Ni1.50 O16'
_cod_database_code               4118052
loop_
_symmetry_equiv_pos_as_xyz
'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
Ni1 Ni 0.74939(5) 0.66744(6) 0.59364(5) 0.0452(2) Uani 1 1 d .
Mn1 Mn 0.5000 0.5000 0.5000 0.0283(3) Uani 1 2 d S
O1 O 0.5549(2) 0.6271(3) 1.4646(2) 0.0399(9) Uani 1 1 d .
C1 C 0.6287(4) 0.6890(4) 1.4611(3) 0.0320(12) Uani 1 1 d .
Ni2 Ni 0.0000 0.5000 0.5000 0.0443(3) Uani 1 2 d S
O2 O 0.7097(2) 0.7118(3) 1.5008(2) 0.0398(9) Uani 1 1 d .
C2 C 0.6187(4) 0.7414(5) 1.4026(3) 0.0443(15) Uani 1 1 d .
O3 O 0.5958(3) 0.8808(3) 1.2374(2) 0.0529(11) Uani 1 1 d .
C3 C 0.6964(4) 0.8136(5) 1.3952(4) 0.0516(16) Uani 1 1 d .
H3 H 0.7577 0.8322 1.4281 0.062 Uiso 1 1 calc R
O4 O 0.5391(2) 1.0607(3) 1.2453(2) 0.0450(9) Uani 1 1 d .
C4 C 0.6862(4) 0.8583(5) 1.3414(4) 0.0573(18) Uani 1 1 d .
H4 H 0.7407 0.9104 1.3388 0.069 Uiso 1 1 calc R
O5 O 0.7678(2) 1.5512(3) 1.4958(2) 0.0405(9) Uani 1 1 d .
C5 C 0.5978(4) 0.8296(4) 1.2898(4) 0.0416(14) Uani 1 1 d .
O6 O 0.6365(2) 1.5054(3) 1.5253(2) 0.0365(9) Uani 1 1 d .
C6 C 0.5222(4) 0.7604(5) 1.2973(4) 0.0512(16) Uani 1 1 d .
H6 H 0.4612 0.7420 1.2638 0.061 Uiso 1 1 calc R
O7 O 0.5842(3) 0.9255(3) 1.0074(2) 0.0528(11) Uani 1 1 d .
C7 C 0.5308(4) 0.7153(5) 1.3525(4) 0.0462(15) Uani 1 1 d .
H7 H 0.4759 0.6654 1.3564 0.055 Uiso 1 1 calc R
O8 O 0.7004(3) 0.7355(3) 0.6825(2) 0.0541(11) Uani 1 1 d .
C8 C 0.5058(4) 0.8553(4) 1.1839(3) 0.0399(13) Uani 1 1 d .
H8A H 0.4716 0.8760 1.2225 0.048 Uiso 1 1 calc R
H8B H 0.4670 0.7792 1.1450 0.048 Uiso 1 1 calc R
O9 O 0.5505(2) 0.6069(3) 0.6387(2) 0.0402(9) Uani 1 1 d .
C9 C 0.5250(4) 0.9154(4) 1.1279(3) 0.0380(13) Uani 1 1 d .
O10 O 0.8839(3) 0.7983(4) 0.6341(3) 0.0930(16) Uani 1 1 d .
C10 C 0.5871(4) 1.0336(4) 1.1874(3) 0.0389(13) Uani 1 1 d .
H10A H 0.6498 1.0505 1.2224 0.047 Uiso 1 1 calc R
H10B H 0.5959 1.0725 1.1506 0.047 Uiso 1 1 calc R
O11 O 0.8055(4) 0.6291(5) 0.6896(3) 0.1045(18) Uani 1 1 d .
C11 C 0.5810(4) 1.1640(4) 1.3029(3) 0.0365(13) Uani 1 1 d .
O12 O 0.3764(3) 0.7823(3) 1.0125(2) 0.0502(10) Uani 1 1 d .
C12 C 0.6620(4) 1.2407(4) 1.3059(3) 0.0384(13) Uani 1 1 d .
H12 H 0.6947 1.2238 1.2674 0.046 Uiso 1 1 calc R
O13 O 0.0528(3) 0.6985(4) 0.6933(3) 0.0676(13) Uani 1 1 d .
C13 C 0.6974(3) 1.3455(4) 1.3662(3) 0.0341(13) Uani 1 1 d .
H13 H 0.7541 1.3993 1.3684 0.041 Uiso 1 1 calc R
O14 O 0.0745(2) 0.5614(3) 0.6335(2) 0.0531(11) Uani 1 1 d .
C14 C 0.6500(3) 1.3706(4) 1.4224(3) 0.0339(13) Uani 1 1 d .
O15 O 0.1153(3) 0.6088(4) 0.4829(3) 0.0689(13) Uani 1 1 d .
C15 C 0.5652(4) 1.2904(5) 1.4172(3) 0.0392(14) Uani 1 1 d .
H15 H 0.5318 1.3068 1.4551 0.047 Uiso 1 1 calc R
O16 O 0.0487(2) 0.3969(3) 0.4764(2) 0.0509(10) Uani 1 1 d .
C16 C 0.5304(4) 1.1888(4) 1.3576(4) 0.0422(14) Uani 1 1 d .
H16 H 0.4721 1.1351 1.3532 0.051 Uiso 1 1 calc R
C17 C 0.6873(4) 1.4803(5) 1.4836(3) 0.0363(13) Uani 1 1 d .
C18 C 0.5769(4) 0.8784(5) 1.0681(3) 0.0506(16) Uani 1 1 d .
H18A H 0.6405 0.9001 1.1053 0.061 Uiso 1 1 calc R
H18B H 0.5412 0.8012 1.0345 0.061 Uiso 1 1 calc R
C19 C 0.5939(5) 0.8693(5) 0.9323(4) 0.0453(15) Uani 1 1 d .
C20 C 0.6800(5) 0.9021(5) 0.9201(4) 0.075(2) Uani 1 1 d .
H20 H 0.7343 0.9643 0.9649 0.090 Uiso 1 1 calc R
C21 C 0.6870(5) 0.8444(6) 0.8423(4) 0.078(2) Uani 1 1 d .
H21 H 0.7468 0.8681 0.8347 0.093 Uiso 1 1 calc R
C22 C 0.6125(4) 0.7559(4) 0.7771(3) 0.0380(13) Uani 1 1 d .
C23 C 0.5266(4) 0.7244(5) 0.7876(3) 0.0527(17) Uani 1 1 d .
H23 H 0.4728 0.6635 0.7410 0.063 Uiso 1 1 calc R
C24 C 0.5159(4) 0.7789(5) 0.8642(4) 0.0562(17) Uani 1 1 d .
H24 H 0.4555 0.7548 0.8705 0.067 Uiso 1 1 calc R
C25 C 0.6216(5) 0.6939(5) 0.6926(4) 0.0449(15) Uani 1 1 d .
C26 C 0.4317(4) 0.8921(4) 1.0712(3) 0.0410(14) Uani 1 1 d .
H26A H 0.3975 0.9125 1.1101 0.049 Uiso 1 1 calc R
H26B H 0.4427 0.9328 1.0359 0.049 Uiso 1 1 calc R
C27 C 0.3031(4) 0.7506(4) 0.9401(4) 0.0448(14) Uani 1 1 d .
C28 C 0.2639(4) 0.6509(5) 0.8744(3) 0.0508(16) Uani 1 1 d .
H28 H 0.2864 0.6066 0.8822 0.061 Uiso 1 1 calc R
C29 C 0.1931(4) 0.6145(5) 0.7980(4) 0.0469(15) Uani 1 1 d .
H29 H 0.1661 0.5447 0.7539 0.056 Uiso 1 1 calc R
C30 C 0.1597(4) 0.6780(5) 0.7835(4) 0.0465(15) Uani 1 1 d .
C31 C 0.1965(4) 0.7758(5) 0.8522(3) 0.0494(16) Uani 1 1 d .
H31 H 0.1714 0.8187 0.8462 0.059 Uiso 1 1 calc R
C32 C 0.2668(4) 0.8128(5) 0.9276(4) 0.0500(15) Uani 1 1 d .
H32 H 0.2919 0.8817 0.9727 0.060 Uiso 1 1 calc R
C33 C 0.0901(4) 0.6425(5) 0.6956(4) 0.0476(16) Uani 1 1 d .
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'
O O 0.0106 0.0060 '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'
Ni Ni 0.3393 1.1124 '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
O8 Ni1 O2 95.14(15) . 1_554
O8 Ni1 O10 97.91(18) . .
O2 Ni1 O10 85.95(17) 1_554 .
O8 Ni1 O11 88.42(18) . .
O2 Ni1 O11 173.9(2) 1_554 .
O10 Ni1 O11 88.6(2) . .
O8 Ni1 O6 103.09(15) . 1_544
O2 Ni1 O6 96.38(13) 1_554 1_544
O10 Ni1 O6 158.55(17) . 1_544
O11 Ni1 O6 87.66(18) . 1_544
O8 Ni1 O5 162.60(16) . 1_544
O2 Ni1 O5 91.79(13) 1_554 1_544
O10 Ni1 O5 98.48(17) . 1_544
O11 Ni1 O5 86.20(16) . 1_544
O6 Ni1 O5 60.20(13) 1_544 1_544
O1 Mn1 O1 180.000(1) 1_554 2_667
O1 Mn1 O9 88.87(13) 1_554 2_666
O1 Mn1 O9 91.13(14) 2_667 2_666
O1 Mn1 O9 91.13(13) 1_554 .
O1 Mn1 O9 88.87(13) 2_667 .
O9 Mn1 O9 180.000(1) 2_666 .
O1 Mn1 O6 90.81(12) 1_554 1_544
O1 Mn1 O6 89.19(12) 2_667 1_544
O9 Mn1 O6 93.04(13) 2_666 1_544
O9 Mn1 O6 86.96(13) . 1_544
O1 Mn1 O6 89.19(12) 1_554 2_677
O1 Mn1 O6 90.81(12) 2_667 2_677
O9 Mn1 O6 86.96(13) 2_666 2_677
O9 Mn1 O6 93.04(13) . 2_677
O6 Mn1 O6 180.0 1_544 2_677
C1 O1 Mn1 140.9(3) . 1_556
O1 C1 O2 126.2(4) . .
O1 C1 C2 116.0(5) . .
O2 C1 C2 117.8(5) . .
O16 Ni2 O16 180.000(1) . 2_566
O16 Ni2 O14 92.50(16) . 2_566
O16 Ni2 O14 87.50(16) 2_566 2_566
O16 Ni2 O14 87.50(16) . .
O16 Ni2 O14 92.50(16) 2_566 .
O14 Ni2 O14 180.000(1) 2_566 .
O16 Ni2 O15 91.96(15) . .
O16 Ni2 O15 88.04(15) 2_566 .
O14 Ni2 O15 89.01(15) 2_566 .
O14 Ni2 O15 90.99(15) . .
O16 Ni2 O15 88.04(15) . 2_566
O16 Ni2 O15 91.96(15) 2_566 2_566
O14 Ni2 O15 90.99(15) 2_566 2_566
O14 Ni2 O15 89.01(15) . 2_566
O15 Ni2 O15 180.0(4) . 2_566
C1 O2 Ni1 128.0(3) . 1_556
C3 C2 C7 118.1(5) . .
C3 C2 C1 121.1(5) . .
C7 C2 C1 120.8(5) . .
C5 O3 C8 118.3(4) . .
C4 C3 C2 120.3(5) . .
C11 O4 C10 116.2(4) . .
C3 C4 C5 121.1(5) . .
C17 O5 Ni1 90.4(3) . 1_566
C6 C5 O3 125.0(5) . .
C6 C5 C4 118.8(5) . .
O3 C5 C4 116.2(5) . .
C17 O6 Ni1 90.6(3) . 1_566
C17 O6 Mn1 140.9(3) . 1_566
Ni1 O6 Mn1 109.07(15) 1_566 1_566
C5 C6 C7 121.0(5) . .
C19 O7 C18 111.6(4) . .
C6 C7 C2 120.6(5) . .
C25 O8 Ni1 128.0(4) . .
O3 C8 C9 106.7(4) . .
C25 O9 Mn1 137.7(3) . .
C26 C9 C8 108.6(4) . .
C26 C9 C10 109.5(4) . .
C8 C9 C10 111.0(4) . .
C26 C9 C18 110.6(4) . .
C8 C9 C18 107.9(4) . .
C10 C9 C18 109.2(4) . .
O4 C10 C9 106.3(4) . .
C12 C11 O4 124.7(5) . .
C12 C11 C16 120.3(5) . .
O4 C11 C16 114.8(5) . .
C27 O12 C26 117.4(4) . .
C11 C12 C13 119.8(5) . .
C14 C13 C12 120.4(5) . .
C33 O14 Ni2 127.9(4) . .
C13 C14 C15 119.1(5) . .
C13 C14 C17 119.5(5) . .
C15 C14 C17 121.4(4) . .
C16 C15 C14 120.3(5) . .
C15 C16 C11 120.0(5) . .
O5 C17 O6 118.8(5) . .
O5 C17 C14 121.8(4) . .
O6 C17 C14 119.4(5) . .
O7 C18 C9 107.6(4) . .
O7 C19 C20 121.1(5) . .
O7 C19 C24 120.5(6) . .
C20 C19 C24 118.3(5) . .
C19 C20 C21 119.6(6) . .
C22 C21 C20 122.5(6) . .
C21 C22 C23 118.2(5) . .
C21 C22 C25 121.7(6) . .
C23 C22 C25 120.0(5) . .
C22 C23 C24 121.5(5) . .
C23 C24 C19 119.8(6) . .
O9 C25 O8 126.1(5) . .
O9 C25 C22 117.7(5) . .
O8 C25 C22 116.2(5) . .
O12 C26 C9 109.0(4) . .
O12 C27 C28 117.1(5) . .
O12 C27 C32 124.8(5) . .
C28 C27 C32 118.1(5) . .
C29 C28 C27 120.9(5) . .
C28 C29 C30 121.1(6) . .
C31 C30 C29 116.9(5) . .
C31 C30 C33 122.0(6) . .
C29 C30 C33 121.0(6) . .
C32 C31 C30 122.3(6) . .
C31 C32 C27 120.4(6) . .
O14 C33 O13 127.5(5) . .
O14 C33 C30 116.4(6) . .
O13 C33 C30 116.1(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O8 2.024(4) .
Ni1 O2 2.038(3) 1_554
Ni1 O10 2.105(5) .
Ni1 O11 2.121(5) .
Ni1 O6 2.170(4) 1_544
Ni1 O5 2.187(4) 1_544
Mn1 O1 2.141(3) 1_554
Mn1 O1 2.141(3) 2_667
Mn1 O9 2.150(3) 2_666
Mn1 O9 2.150(3) .
Mn1 O6 2.203(3) 1_544
Mn1 O6 2.203(3) 2_677
O1 C1 1.228(5) .
O1 Mn1 2.141(3) 1_556
C1 O2 1.246(6) .
C1 C2 1.508(7) .
Ni2 O16 2.049(4) .
Ni2 O16 2.049(4) 2_566
Ni2 O14 2.062(3) 2_566
Ni2 O14 2.062(3) .
Ni2 O15 2.100(4) .
Ni2 O15 2.100(4) 2_566
O2 Ni1 2.038(3) 1_556
C2 C3 1.369(7) .
C2 C7 1.381(7) .
O3 C5 1.381(6) .
O3 C8 1.434(6) .
C3 C4 1.347(7) .
O4 C11 1.364(6) .
O4 C10 1.421(6) .
C4 C5 1.384(7) .
O5 C17 1.258(6) .
O5 Ni1 2.187(4) 1_566
C5 C6 1.329(7) .
O6 C17 1.281(6) .
O6 Ni1 2.170(3) 1_566
O6 Mn1 2.203(3) 1_566
C6 C7 1.365(7) .
O7 C19 1.362(6) .
O7 C18 1.439(6) .
O8 C25 1.262(6) .
C8 C9 1.519(7) .
O9 C25 1.258(7) .
C9 C26 1.515(7) .
C9 C10 1.536(7) .
C9 C18 1.549(7) .
C11 C12 1.355(7) .
C11 C16 1.411(7) .
O12 C27 1.362(6) .
O12 C26 1.436(6) .
C12 C13 1.409(7) .
O13 C33 1.278(7) .
C13 C14 1.384(7) .
O14 C33 1.242(7) .
C14 C15 1.405(7) .
C14 C17 1.466(7) .
C15 C16 1.370(7) .
C19 C20 1.376(8) .
C19 C24 1.392(8) .
C20 C21 1.381(9) .
C21 C22 1.342(8) .
C22 C23 1.361(7) .
C22 C25 1.509(7) .
C23 C24 1.380(8) .
C27 C28 1.371(8) .
C27 C32 1.399(8) .
C28 C29 1.363(7) .
C29 C30 1.395(8) .
C30 C31 1.376(8) .
C30 C33 1.495(7) .
C31 C32 1.344(7) .
