#------------------------------------------------------------------------------
#$Date: 2016-03-21 01:21:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178377 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/16/4001626.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_4001626
loop_
_publ_author_name
'Yao, Ru-Xin'
'Xu, Xia'
'Zhang, Xian-Ming'
_publ_section_title
;
 Magnetic Modulation and Cation-Exchange in a Series of Isostructural
 (4,8)-Connected Metal--Organic Frameworks with Butterfly-like
 [M4(OH)2(RCO2)8] Building Units
;
_journal_issue                   2
_journal_name_full               'Chemistry of Materials'
_journal_page_first              303
_journal_paper_doi               10.1021/cm202876r
_journal_volume                  24
_journal_year                    2012
_chemical_formula_sum            'C18 H19 Co1.66 N Ni0.34 O11'
_chemical_formula_weight         543.09
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 110.6380(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.5674(5)
_cell_length_b                   10.7942(4)
_cell_length_c                   14.6837(5)
_cell_measurement_reflns_used    8360
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.47
_cell_measurement_theta_min      2.39
_cell_volume                     2012.42(13)
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SAINT (Bruker, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Apex CCD Diffractometer'
_diffrn_measurement_method       'φ and ω 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  0.0161
_diffrn_reflns_av_sigmaI/netI    0.0179
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12240
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         2.40
_exptl_absorpt_coefficient_mu    1.750
_exptl_absorpt_correction_T_max  0.8584
_exptl_absorpt_correction_T_min  0.6891
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1997'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.776
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       sheet
_exptl_crystal_F_000             1085
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.728
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4384
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0469P)²+0.9761P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0769
_reflns_number_gt                4081
_reflns_number_total             4384
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm202876r_si_002.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4001626
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, 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
Co1 Co 0.409875(17) 0.90280(2) 0.461419(15) 0.01636(8) Uani 0.83 1 d P
Ni1 Ni 0.409875(17) 0.90280(2) 0.461419(15) 0.01636(8) Uani 0.17 1 d P
Co2 Co 0.504017(17) 1.01028(2) 0.292216(15) 0.01591(8) Uani 0.83 1 d P
Ni2 Ni 0.504017(17) 1.01028(2) 0.292216(15) 0.01591(8) Uani 0.17 1 d P
N1 N 0.25195(17) 0.0385(2) 0.05500(16) 0.0514(6) Uani 1 1 d .
H1D H 0.2899 -0.0081 0.1062 0.062 Uiso 1 1 calc R
H1E H 0.2717 0.1179 0.0691 0.062 Uiso 1 1 calc R
O1 O 0.30272(10) 1.03092(12) 0.37225(10) 0.0248(3) Uani 1 1 d .
O2 O 0.38901(10) 1.13589(12) 0.29179(10) 0.0240(3) Uani 1 1 d .
O3 O 0.38502(11) 1.40408(13) 0.23917(11) 0.0298(3) Uani 1 1 d .
O4 O 0.31160(12) 1.28409(15) 0.10882(10) 0.0345(3) Uani 1 1 d .
O5 O -0.37885(10) 1.14649(13) 0.34146(9) 0.0270(3) Uani 1 1 d .
O6 O -0.28486(10) 1.15291(13) 0.50127(9) 0.0259(3) Uani 1 1 d .
O7 O -0.36649(10) 1.27700(12) 0.15425(9) 0.0222(3) Uani 1 1 d .
O8 O -0.37066(10) 1.39555(12) 0.27859(9) 0.0218(3) Uani 1 1 d .
O9 O 0.53869(9) 0.95877(11) 0.43211(8) 0.0174(2) Uani 1 1 d .
C1 C 0.1404(2) 0.0268(3) 0.0419(3) 0.0752(11) Uani 1 1 d .
H1A H 0.1296 0.0531 0.1001 0.113 Uiso 1 1 calc R
H1B H 0.1191 -0.0581 0.0286 0.113 Uiso 1 1 calc R
H1C H 0.0994 0.0776 -0.0117 0.113 Uiso 1 1 calc R
C2 C 0.2769(3) 0.0000(4) -0.0318(3) 0.0812(12) Uani 1 1 d .
H2A H 0.3511 0.0095 -0.0184 0.122 Uiso 1 1 calc R
H2B H 0.2384 0.0509 -0.0863 0.122 Uiso 1 1 calc R
H2C H 0.2574 -0.0851 -0.0466 0.122 Uiso 1 1 calc R
C3 C 0.31196(13) 1.11703(16) 0.31935(12) 0.0183(3) Uani 1 1 d .
C4 C 0.22361(13) 1.20968(17) 0.28526(13) 0.0203(3) Uani 1 1 d .
C5 C 0.13904(14) 1.19568(17) 0.31758(13) 0.0231(4) Uani 1 1 d .
H5A H 0.1393 1.1297 0.3584 0.028 Uiso 1 1 calc R
C6 C 0.05451(13) 1.27732(18) 0.29057(13) 0.0227(4) Uani 1 1 d .
C7 C 0.05677(15) 1.37567(19) 0.22936(15) 0.0298(4) Uani 1 1 d .
H7A H 0.0013 1.4320 0.2102 0.036 Uiso 1 1 calc R
C8 C 0.14036(15) 1.39052(19) 0.19682(16) 0.0296(4) Uani 1 1 d .
H8A H 0.1401 1.4567 0.1562 0.036 Uiso 1 1 calc R
C9 C 0.22479(14) 1.30800(17) 0.22402(13) 0.0225(4) Uani 1 1 d .
C10 C 0.31508(14) 1.33177(17) 0.18769(13) 0.0227(4) Uani 1 1 d .
C11 C -0.03432(13) 1.25856(17) 0.32627(13) 0.0213(4) Uani 1 1 d .
C12 C -0.01754(14) 1.20296(18) 0.41656(13) 0.0234(4) Uani 1 1 d .
H12A H 0.0506 1.1822 0.4563 0.028 Uiso 1 1 calc R
C13 C -0.10101(14) 1.17834(18) 0.44764(13) 0.0221(4) Uani 1 1 d .
H13A H -0.0885 1.1411 0.5078 0.027 Uiso 1 1 calc R
C14 C -0.20336(13) 1.20915(16) 0.38914(12) 0.0183(3) Uani 1 1 d .
C15 C -0.22056(13) 1.27047(16) 0.30119(12) 0.0178(3) Uani 1 1 d .
C16 C -0.13727(14) 1.29338(17) 0.26935(13) 0.0214(4) Uani 1 1 d .
H16A H -0.1499 1.3322 0.2097 0.026 Uiso 1 1 calc R
C17 C -0.32876(13) 1.31638(16) 0.24022(12) 0.0177(3) Uani 1 1 d .
C18 C -0.29668(13) 1.16615(16) 0.41328(12) 0.0184(3) Uani 1 1 d .
O1W O 0.49698(13) 0.73524(15) 0.54114(11) 0.0394(4) Uani 1 1 d .
O2W O 0.48153(12) 1.09569(16) 0.15150(11) 0.0378(4) 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'
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'
Co Co 0.3494 0.9721 '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
O9 Co1 O6 176.92(5) . 3_576
O9 Co1 O7 92.17(5) . 2_545
O6 Co1 O7 90.23(5) 3_576 2_545
O9 Co1 O9 82.01(5) . 3_676
O6 Co1 O9 95.69(5) 3_576 3_676
O7 Co1 O9 173.34(5) 2_545 3_676
O9 Co1 O1 97.49(5) . .
O6 Co1 O1 84.46(5) 3_576 .
O7 Co1 O1 89.22(5) 2_545 .
O9 Co1 O1 88.33(5) 3_676 .
O9 Co1 O1W 90.91(6) . .
O6 Co1 O1W 87.56(6) 3_576 .
O7 Co1 O1W 81.16(5) 2_545 .
O9 Co1 O1W 102.08(5) 3_676 .
O1 Co1 O1W 167.48(6) . .
O9 Co2 O2 95.10(5) . .
O9 Co2 O3 98.47(5) . 2_645
O2 Co2 O3 166.19(6) . 2_645
O9 Co2 O5 88.04(5) . 1_655
O2 Co2 O5 91.19(5) . 1_655
O3 Co2 O5 86.72(6) 2_645 1_655
O9 Co2 O8 100.91(5) . 2_545
O2 Co2 O8 82.51(5) . 2_545
O3 Co2 O8 97.38(5) 2_645 2_545
O5 Co2 O8 169.44(5) 1_655 2_545
O9 Co2 O2W 169.95(6) . .
O2 Co2 O2W 82.33(6) . .
O3 Co2 O2W 83.86(6) 2_645 .
O5 Co2 O2W 82.33(5) 1_655 .
O8 Co2 O2W 88.42(5) 2_545 .
C1 N1 C2 113.6(3) . .
C3 O1 Co1 132.95(12) . .
C3 O2 Co2 127.06(12) . .
C10 O3 Ni2 131.70(13) . 2_655
C10 O3 Co2 131.70(13) . 2_655
Ni2 O3 Co2 0.000(15) 2_655 2_655
C18 O5 Ni2 138.57(12) . 1_455
C18 O5 Co2 138.57(12) . 1_455
Ni2 O5 Co2 0.000(10) 1_455 1_455
C18 O6 Ni1 119.50(11) . 3_576
C18 O6 Co1 119.50(11) . 3_576
Ni1 O6 Co1 0.000(13) 3_576 3_576
C17 O7 Ni1 119.64(11) . 2
C17 O7 Co1 119.64(11) . 2
Ni1 O7 Co1 0.000(15) 2 2
C17 O8 Ni2 127.75(11) . 2
C17 O8 Co2 127.75(11) . 2
Ni2 O8 Co2 0.000(9) 2 2
Co2 O9 Co1 112.84(5) . .
Co2 O9 Ni1 117.38(6) . 3_676
Co1 O9 Ni1 97.99(5) . 3_676
Co2 O9 Co1 117.38(6) . 3_676
Co1 O9 Co1 97.99(5) . 3_676
Ni1 O9 Co1 0.000(10) 3_676 3_676
O1 C3 O2 126.62(16) . .
O1 C3 C4 117.38(15) . .
O2 C3 C4 116.00(15) . .
C9 C4 C5 119.94(16) . .
C9 C4 C3 122.10(15) . .
C5 C4 C3 117.96(16) . .
C6 C5 C4 121.95(17) . .
C5 C6 C7 117.54(17) . .
C5 C6 C11 120.20(16) . .
C7 C6 C11 122.26(16) . .
C8 C7 C6 121.01(17) . .
C7 C8 C9 121.12(17) . .
C8 C9 C4 118.43(16) . .
C8 C9 C10 118.29(16) . .
C4 C9 C10 123.25(16) . .
O4 C10 O3 125.90(17) . .
O4 C10 C9 118.85(17) . .
O3 C10 C9 115.16(16) . .
C12 C11 C16 118.35(16) . .
C12 C11 C6 120.72(15) . .
C16 C11 C6 120.91(16) . .
C13 C12 C11 120.98(16) . .
C12 C13 C14 120.25(16) . .
C13 C14 C15 119.31(15) . .
C13 C14 C18 121.39(15) . .
C15 C14 C18 118.98(15) . .
C16 C15 C14 120.36(15) . .
C16 C15 C17 118.61(15) . .
C14 C15 C17 121.01(15) . .
C15 C16 C11 120.61(16) . .
O7 C17 O8 126.04(16) . .
O7 C17 C15 116.84(15) . .
O8 C17 C15 117.02(15) . .
O6 C18 O5 126.93(16) . .
O6 C18 C14 117.78(15) . .
O5 C18 C14 115.29(15) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O9 2.0335(12) .
Co1 O6 2.0478(13) 3_576
Co1 O7 2.0905(12) 2_545
Co1 O9 2.0964(12) 3_676
Co1 O1 2.0973(13) .
Co1 O1W 2.2501(16) .
Co2 O9 2.0171(12) .
Co2 O2 2.0655(13) .
Co2 O3 2.0693(13) 2_645
Co2 O5 2.0976(13) 1_655
Co2 O8 2.1360(12) 2_545
Co2 O2W 2.1836(15) .
N1 C1 1.462(4) .
N1 C2 1.488(4) .
O1 C3 1.246(2) .
O2 C3 1.263(2) .
O3 C10 1.255(2) .
O3 Ni2 2.0693(13) 2_655
O3 Co2 2.0693(13) 2_655
O4 C10 1.253(2) .
O5 C18 1.253(2) .
O5 Ni2 2.0976(13) 1_455
O5 Co2 2.0976(13) 1_455
O6 C18 1.253(2) .
O6 Ni1 2.0478(13) 3_576
O6 Co1 2.0478(13) 3_576
O7 C17 1.257(2) .
O7 Ni1 2.0905(12) 2
O7 Co1 2.0905(12) 2
O8 C17 1.263(2) .
O8 Ni2 2.1360(12) 2
O8 Co2 2.1360(12) 2
O9 Ni1 2.0964(12) 3_676
O9 Co1 2.0964(12) 3_676
C3 C4 1.505(2) .
C4 C9 1.395(2) .
C4 C5 1.396(2) .
C5 C6 1.389(3) .
C6 C7 1.398(3) .
C6 C11 1.488(2) .
C7 C8 1.386(3) .
C8 C9 1.394(3) .
C9 C10 1.521(2) .
C11 C12 1.399(3) .
C11 C16 1.403(2) .
C12 C13 1.388(2) .
C13 C14 1.391(2) .
C14 C15 1.396(2) .
C14 C18 1.503(2) .
C15 C16 1.389(2) .
C15 C17 1.509(2) .
