#------------------------------------------------------------------------------
#$Date: 2016-03-21 01:21:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178377 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/16/4001627.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_4001627
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 Co1.09 N Ni0.91 O11'
_chemical_formula_weight         542.96
_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                 110.6310(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.5146(8)
_cell_length_b                   10.7692(6)
_cell_length_c                   14.6278(8)
_cell_measurement_reflns_used    1823
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      23.31
_cell_measurement_theta_min      2.40
_cell_volume                     1992.4(2)
_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  0.0502
_diffrn_reflns_av_sigmaI/netI    0.0654
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12082
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    1.831
_exptl_absorpt_correction_T_max  0.8981
_exptl_absorpt_correction_T_min  0.7582
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1997'
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    1.793
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       sheet
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4353
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0549P)²+0.0817P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.1096
_reflns_number_gt                3240
_reflns_number_total             4353
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm202876r_si_002.cif
_cod_data_source_block           3
_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               4001627
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 0.41043(3) 0.90418(4) 0.46172(3) 0.01539(13) Uani 0.55 1 d P
Ni1 Ni 0.41043(3) 0.90418(4) 0.46172(3) 0.01539(13) Uani 0.45 1 d P
Co2 Co 0.50384(3) 1.01050(4) 0.29221(3) 0.01478(13) Uani 0.55 1 d P
Ni2 Ni 0.50384(3) 1.01050(4) 0.29221(3) 0.01478(13) Uani 0.45 1 d P
N1 N 0.2533(3) 0.0378(4) 0.0545(3) 0.0503(11) Uani 1 1 d .
H1D H 0.2912 -0.0091 0.1058 0.060 Uiso 1 1 calc R
H1E H 0.2737 0.1172 0.0685 0.060 Uiso 1 1 calc R
O1 O 0.30463(19) 1.0310(2) 0.37377(18) 0.0240(6) Uani 1 1 d .
O2 O 0.38991(18) 1.1350(2) 0.29059(18) 0.0226(6) Uani 1 1 d .
O3 O 0.3862(2) 1.4042(2) 0.23847(19) 0.0284(6) Uani 1 1 d .
O4 O 0.3126(2) 1.2845(3) 0.10776(19) 0.0332(7) Uani 1 1 d .
O5 O -0.37990(19) 1.1458(2) 0.34031(18) 0.0253(6) Uani 1 1 d .
O6 O -0.28615(18) 1.1519(2) 0.50127(17) 0.0240(6) Uani 1 1 d .
O7 O -0.36646(18) 1.2770(2) 0.15290(17) 0.0221(6) Uani 1 1 d .
O8 O -0.37184(18) 1.3956(2) 0.27768(17) 0.0204(6) Uani 1 1 d .
O9 O 0.53807(17) 0.9595(2) 0.43152(16) 0.0175(5) Uani 1 1 d .
C1 C 0.1409(4) 0.0271(5) 0.0416(5) 0.0727(18) Uani 1 1 d .
H1A H 0.1305 0.0537 0.1002 0.109 Uiso 1 1 calc R
H1B H 0.1188 -0.0577 0.0281 0.109 Uiso 1 1 calc R
H1C H 0.0999 0.0785 -0.0120 0.109 Uiso 1 1 calc R
C2 C 0.2778(5) -0.0017(6) -0.0333(4) 0.077(2) Uani 1 1 d .
H2A H 0.3522 0.0075 -0.0203 0.115 Uiso 1 1 calc R
H2B H 0.2389 0.0491 -0.0881 0.115 Uiso 1 1 calc R
H2C H 0.2581 -0.0871 -0.0478 0.115 Uiso 1 1 calc R
C3 C 0.3130(3) 1.1172(3) 0.3191(2) 0.0183(7) Uani 1 1 d .
C4 C 0.2248(3) 1.2086(3) 0.2853(3) 0.0189(8) Uani 1 1 d .
C5 C 0.1398(3) 1.1948(4) 0.3178(3) 0.0226(8) Uani 1 1 d .
H5A H 0.1399 1.1287 0.3587 0.027 Uiso 1 1 calc R
C6 C 0.0549(3) 1.2774(4) 0.2906(3) 0.0217(8) Uani 1 1 d .
C7 C 0.0577(3) 1.3754(4) 0.2295(3) 0.0284(9) Uani 1 1 d .
H7A H 0.0026 1.4326 0.2108 0.034 Uiso 1 1 calc R
C8 C 0.1412(3) 1.3894(4) 0.1963(3) 0.0289(9) Uani 1 1 d .
H8A H 0.1405 1.4549 0.1546 0.035 Uiso 1 1 calc R
C9 C 0.2257(3) 1.3075(4) 0.2240(3) 0.0208(8) Uani 1 1 d .
C10 C 0.3163(3) 1.3320(4) 0.1870(3) 0.0223(8) Uani 1 1 d .
C11 C -0.0342(3) 1.2580(4) 0.3257(3) 0.0216(8) Uani 1 1 d .
C12 C -0.0177(3) 1.2031(4) 0.4167(3) 0.0221(8) Uani 1 1 d .
H12A H 0.0506 1.1830 0.4571 0.027 Uiso 1 1 calc R
C13 C -0.1018(3) 1.1785(4) 0.4473(3) 0.0219(8) Uani 1 1 d .
H13A H -0.0894 1.1413 0.5077 0.026 Uiso 1 1 calc R
C14 C -0.2037(3) 1.2085(3) 0.3890(2) 0.0176(7) Uani 1 1 d .
C15 C -0.2215(3) 1.2705(3) 0.3003(2) 0.0183(8) Uani 1 1 d .
C16 C -0.1374(3) 1.2932(3) 0.2692(3) 0.0212(8) Uani 1 1 d .
H16A H -0.1498 1.3326 0.2097 0.025 Uiso 1 1 calc R
C17 C -0.3292(3) 1.3165(3) 0.2393(3) 0.0186(8) Uani 1 1 d .
C18 C -0.2980(3) 1.1655(3) 0.4125(3) 0.0180(7) Uani 1 1 d .
O1W O 0.4972(2) 0.7396(3) 0.54086(19) 0.0363(7) Uani 1 1 d .
O2W O 0.4835(2) 1.0922(3) 0.15109(19) 0.0369(8) 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 177.36(9) . 3_576
O9 Co1 O1 97.24(10) . .
O6 Co1 O1 84.64(10) 3_576 .
O9 Co1 O9 82.52(9) . 3_676
O6 Co1 O9 95.70(10) 3_576 3_676
O1 Co1 O9 88.64(10) . 3_676
O9 Co1 O7 92.38(9) . 2_545
O6 Co1 O7 89.48(10) 3_576 2_545
O1 Co1 O7 89.69(10) . 2_545
O9 Co1 O7 174.39(9) 3_676 2_545
O9 Co1 O1W 90.86(10) . .
O6 Co1 O1W 87.58(10) 3_576 .
O1 Co1 O1W 167.90(11) . .
O9 Co1 O1W 101.37(10) 3_676 .
O7 Co1 O1W 80.97(10) 2_545 .
O9 Co2 O2 95.46(10) . .
O9 Co2 O3 98.32(10) . 2_645
O2 Co2 O3 166.03(10) . 2_645
O9 Co2 O5 88.37(9) . 1_655
O2 Co2 O5 91.18(10) . 1_655
O3 Co2 O5 86.90(11) 2_645 1_655
O9 Co2 O8 100.65(9) . 2_545
O2 Co2 O8 82.76(10) . 2_545
O3 Co2 O8 96.92(10) 2_645 2_545
O5 Co2 O8 169.54(10) 1_655 2_545
O9 Co2 O2W 170.45(10) . .
O2 Co2 O2W 83.11(11) . .
O3 Co2 O2W 82.92(11) 2_645 .
O5 Co2 O2W 82.23(10) 1_655 .
O8 Co2 O2W 88.57(10) 2_545 .
C1 N1 C2 113.6(4) . .
C3 O1 Co1 133.4(2) . .
C3 O2 Co2 127.1(2) . .
C10 O3 Ni2 132.0(2) . 2_655
C10 O3 Co2 132.0(2) . 2_655
Ni2 O3 Co2 0.00(3) 2_655 2_655
C18 O5 Ni2 138.2(2) . 1_455
C18 O5 Co2 138.2(2) . 1_455
Ni2 O5 Co2 0.000(19) 1_455 1_455
C18 O6 Ni1 119.5(2) . 3_576
C18 O6 Co1 119.5(2) . 3_576
Ni1 O6 Co1 0.00(3) 3_576 3_576
C17 O7 Ni1 119.1(2) . 2
C17 O7 Co1 119.1(2) . 2
Ni1 O7 Co1 0.000(19) 2 2
C17 O8 Ni2 128.2(2) . 2
C17 O8 Co2 128.2(2) . 2
Ni2 O8 Co2 0.000(18) 2 2
Co2 O9 Co1 113.31(10) . .
Co2 O9 Ni1 117.91(12) . 3_676
Co1 O9 Ni1 97.48(9) . 3_676
Co2 O9 Co1 117.91(12) . 3_676
Co1 O9 Co1 97.48(9) . 3_676
Ni1 O9 Co1 0.00(2) 3_676 3_676
O1 C3 O2 126.3(3) . .
O1 C3 C4 117.3(3) . .
O2 C3 C4 116.5(3) . .
C9 C4 C5 119.6(3) . .
C9 C4 C3 122.0(3) . .
C5 C4 C3 118.3(3) . .
C6 C5 C4 121.9(3) . .
C7 C6 C5 117.5(3) . .
C7 C6 C11 122.6(3) . .
C5 C6 C11 119.9(3) . .
C8 C7 C6 121.2(3) . .
C7 C8 C9 121.2(4) . .
C8 C9 C4 118.7(3) . .
C8 C9 C10 117.9(3) . .
C4 C9 C10 123.3(3) . .
O3 C10 O4 125.9(3) . .
O3 C10 C9 115.1(3) . .
O4 C10 C9 118.9(3) . .
C12 C11 C16 117.8(3) . .
C12 C11 C6 120.8(3) . .
C16 C11 C6 121.3(3) . .
C13 C12 C11 120.9(3) . .
C14 C13 C12 120.6(3) . .
C13 C14 C15 119.5(3) . .
C13 C14 C18 121.9(3) . .
C15 C14 C18 118.3(3) . .
C16 C15 C14 119.6(3) . .
C16 C15 C17 118.9(3) . .
C14 C15 C17 121.5(3) . .
C15 C16 C11 121.4(3) . .
O7 C17 O8 126.1(3) . .
O7 C17 C15 116.6(3) . .
O8 C17 C15 117.2(3) . .
O5 C18 O6 127.2(3) . .
O5 C18 C14 115.4(3) . .
O6 C18 C14 117.4(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O9 2.016(2) .
Co1 O6 2.030(2) 3_576
Co1 O1 2.066(2) .
Co1 O9 2.076(2) 3_676
Co1 O7 2.083(2) 2_545
Co1 O1W 2.213(3) .
Co2 O9 2.001(2) .
Co2 O2 2.036(2) .
Co2 O3 2.047(2) 2_645
Co2 O5 2.075(2) 1_655
Co2 O8 2.115(2) 2_545
Co2 O2W 2.171(3) .
N1 C1 1.467(6) .
N1 C2 1.496(7) .
O1 C3 1.257(4) .
O2 C3 1.263(4) .
O3 C10 1.251(4) .
O3 Ni2 2.047(2) 2_655
O3 Co2 2.047(2) 2_655
O4 C10 1.252(4) .
O5 C18 1.250(4) .
O5 Ni2 2.075(2) 1_455
O5 Co2 2.075(2) 1_455
O6 C18 1.259(4) .
O6 Ni1 2.030(2) 3_576
O6 Co1 2.030(2) 3_576
O7 C17 1.258(4) .
O7 Ni1 2.083(2) 2
O7 Co1 2.083(2) 2
O8 C17 1.266(4) .
O8 Ni2 2.115(2) 2
O8 Co2 2.115(2) 2
O9 Ni1 2.076(2) 3_676
O9 Co1 2.076(2) 3_676
C3 C4 1.490(5) .
C4 C9 1.395(5) .
C4 C5 1.397(5) .
C5 C6 1.395(5) .
C6 C7 1.391(5) .
C6 C11 1.481(5) .
C7 C8 1.385(5) .
C8 C9 1.386(5) .
C9 C10 1.525(5) .
C11 C12 1.400(5) .
C11 C16 1.400(5) .
C12 C13 1.387(5) .
C13 C14 1.378(4) .
C14 C15 1.403(5) .
C14 C18 1.505(4) .
C15 C16 1.386(5) .
C15 C17 1.498(5) .
