#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/96/2019669.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2019669
loop_
_publ_author_name
'Harvey, Miguel Angel'
'Suarez, Sebastián'
'Cukiernik, Fabio D.'
'Baggio, Ricardo'
_publ_section_title
;
 The topotactic dehydration of monoclinic
 {[Co(pht)(bpy)(H₂O)₂]·2H₂O}ₙ into orthorhombic
 [Co(pht)(bpy)(H₂O)₂]ₙ (pht is phthalate and bpy is
 4,4'-bipyridine)
;
_journal_coeditor_code           SK3564
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              978
_journal_page_last               982
_journal_paper_doi               10.1107/S2053229614020427
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Co (C8 H4 O4) (C10 H8 N2) (H2 O)2]'
_chemical_formula_moiety         'C18 H16 Co N2 O6'
_chemical_formula_sum            'C18 H16 Co N2 O6'
_chemical_formula_weight         415.27
_chemical_name_systematic
Poly[diaqua(μ₂-benzene-1,2-dicarboxylato-κ²O¹:O²)(μ₂-4,4'-bipyridine-κ²N:N')cobalt(II)]
_space_group_crystal_system      orthorhombic
_space_group_IT_number           31
_space_group_name_Hall           'P 2ac -2'
_space_group_name_H-M_alt        'P m n 21'
_symmetry_space_group_name_Hall  'P 2ac -2'
_symmetry_space_group_name_H-M   'P m n 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL2013
_cell_angle_alpha                90.000
_cell_angle_beta                 90.000
_cell_angle_gamma                90.000
_cell_formula_units_Z            2
_cell_length_a                   7.575(5)
_cell_length_b                   11.410(5)
_cell_length_c                   10.106(5)
_cell_measurement_reflns_used    902
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      24.16
_cell_measurement_theta_min      3.82
_cell_volume                     873.5(8)
_computing_cell_refinement       'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_device_type  'Oxford Gemini S Ultra CCD area-detector'
_diffrn_measurement_method       'ω scans, thick slices'
_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  0.0780
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6622
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.218
_diffrn_reflns_theta_min         3.806
_exptl_absorpt_coefficient_mu    1.021
_exptl_absorpt_correction_T_max  0.74
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Oxford Diffraction, 2009)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             426
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.415
_refine_ls_abs_structure_details
;
Flack (1983); refined as an inversion twin
;
_refine_ls_abs_structure_Flack   0.33(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         1973
_refine_ls_number_restraints     435
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0635
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0843P)²+0.9480P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1484
_refine_ls_wR_factor_ref         0.1705
_reflns_number_gt                1427
_reflns_number_total             1973
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            sk3564sup1.cf
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2019669.cif.'
_cod_database_code               2019669
_cod_database_fobs_code          2019669
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           .2013
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y, z+1/2'
'-x, y, z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co Co1 0.5000 0.11228(9) 0.5146(9) 0.0314(4) Uani d 1 . .
N N12 0.5000 0.3025(5) 0.5173(16) 0.0243(10) Uani d 1 A .
N N22 0.5000 0.9194(5) 0.5078(13) 0.0280(12) Uani d 1 . .
C C32 0.5000 0.5468(6) 0.5227(16) 0.0253(11) Uani d 1 . .
C C82 0.5000 0.6755(6) 0.517(3) 0.0261(11) Uani d 1 A .
O O11 1.016(3) 0.0518(10) 0.6642(17) 0.037(2) Uani d 0.5 A -1
O O21 0.7300(18) 0.1045(11) 0.643(2) 0.0317(17) Uani d 0.5 A -1
O O31 1.004(4) 0.0623(10) 0.3469(15) 0.034(2) Uani d 0.5 A -1
O O41 1.2889(15) 0.1105(12) 0.392(2) 0.0278(18) Uani d 0.5 A -1
C C11 0.9523(16) 0.2410(11) 0.5716(15) 0.0307(12) Uani d 0.5 A -1
C C21 0.8999(15) 0.3482(13) 0.6218(12) 0.0311(14) Uani d 0.5 A -1
H H21A 0.8290 0.3506 0.6969 0.037 Uiso calc 0.5 A -1
C C31 0.951(2) 0.4521(10) 0.5622(17) 0.0311(15) Uani d 0.5 A -1
H H31A 0.9153 0.5232 0.5983 0.037 Uiso calc 0.5 A -1
C C41 1.055(2) 0.4513(12) 0.4496(17) 0.0308(15) Uani d 0.5 A -1
H H41A 1.0880 0.5209 0.4086 0.037 Uiso calc 0.5 A -1
C C51 1.1087(16) 0.3438(13) 0.3996(13) 0.0305(14) Uani d 0.5 A -1
H H51A 1.1793 0.3411 0.3244 0.037 Uiso calc 0.5 A -1
C C61 1.0579(17) 0.2407(10) 0.4607(15) 0.0297(12) Uani d 0.5 A -1
C C71 0.8943(16) 0.1245(14) 0.637(2) 0.0317(14) Uani d 0.5 A -1
C C81 1.1236(17) 0.1252(14) 0.397(2) 0.0289(15) Uani d 0.5 A -1
C C12 0.4313(10) 0.3601(11) 0.6194(14) 0.0253(13) Uani d 0.5 A -2
H H12A 0.3891 0.3172 0.6910 0.030 Uiso calc 0.5 A -2
C C22 0.4198(19) 0.4815(10) 0.6237(15) 0.0255(13) Uani d 0.5 A -2
H H22A 0.3602 0.5188 0.6923 0.031 Uiso calc 0.5 A -2
C C42 0.5555(17) 0.4851(10) 0.4102(14) 0.0255(13) Uani d 0.5 A -2
H H42A 0.5891 0.5249 0.3339 0.031 Uiso calc 0.5 A -2
C C52 0.5595(11) 0.3633(10) 0.4147(14) 0.0253(13) Uani d 0.5 A -2
H H52A 0.6057 0.3228 0.3428 0.030 Uiso calc 0.5 A -2
C C62 0.3551(12) 0.8591(8) 0.4773(10) 0.0284(14) Uani d 0.5 A -2
H H62A 0.2517 0.9000 0.4596 0.034 Uiso calc 0.5 A -2
C C72 0.3522(15) 0.7377(8) 0.4709(18) 0.0275(14) Uani d 0.5 A -2
H H72A 0.2547 0.6983 0.4370 0.033 Uiso calc 0.5 A -2
C C92 0.6590(12) 0.7397(7) 0.529(2) 0.0263(14) Uani d 0.5 A -2
H H92A 0.7672 0.7015 0.5348 0.032 Uiso calc 0.5 A -2
C C102 0.6492(11) 0.8614(8) 0.5333(12) 0.0276(14) Uani d 0.5 A -2
H H10A 0.7502 0.9038 0.5544 0.033 Uiso calc 0.5 A -2
O O1W 0.357(2) 0.1045(12) 0.687(2) 0.027(3) Uani d 0.5 A -2
O O2W 0.659(3) 0.1106(14) 0.333(2) 0.034(4) Uani d 0.5 A -2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3490 0.9720 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O41 Co1 N12 1_455 . 91.0(5)
O1W Co1 N12 . . 91.9(6)
O41 Co1 O21 1_455 . 176.9(4)
N12 Co1 O21 . . 91.9(4)
O1W Co1 O2W . . 176.7(6)
N12 Co1 O2W . . 91.1(6)
O41 Co1 N22 1_455 1_545 88.3(5)
O1W Co1 N22 . 1_545 89.0(6)
N12 Co1 N22 . 1_545 178.9(7)
O21 Co1 N22 . 1_545 88.7(4)
O2W Co1 N22 . 1_545 88.0(6)
C52 N12 C12 . . 118.8(7)
C52 N12 Co1 . . 120.9(9)
C12 N12 Co1 . . 120.2(9)
C62 N22 C102 . . 119.1(6)
C62 N22 Co1 . 1_565 121.6(5)
C102 N22 Co1 . 1_565 119.3(5)
C42 C32 C22 . . 117.0(7)
C42 C32 C82 . . 118.0(13)
C22 C32 C82 . . 124.0(12)
C72 C82 C92 . . 116.5(8)
C72 C82 C32 . . 121.2(7)
C92 C82 C32 . . 120.9(4)
C71 O21 Co1 . . 138.7(17)
C81 O41 Co1 . 1_655 139.2(18)
C61 C11 C21 . . 117.9(11)
C61 C11 C71 . . 120.7(15)
C21 C11 C71 . . 121.4(14)
C11 C21 C31 . . 121.1(8)
C11 C21 H21A . . 119.4
C31 C21 H21A . . 119.4
C41 C31 C21 . . 120.8(10)
C41 C31 H31A . . 119.6
C21 C31 H31A . . 119.6
C31 C41 C51 . . 118.2(11)
C31 C41 H41A . . 120.9
C51 C41 H41A . . 120.9
C61 C51 C41 . . 120.5(8)
C61 C51 H51A . . 119.7
C41 C51 H51A . . 119.7
C11 C61 C51 . . 121.5(9)
C11 C61 C81 . . 121.8(15)
C51 C61 C81 . . 116.8(15)
O11 C71 O21 . . 125.7(15)
O11 C71 C11 . . 116.7(11)
O21 C71 C11 . . 116.9(11)
O41 C81 O31 . . 128.3(19)
O41 C81 C61 . . 116.6(12)
O31 C81 C61 . . 114.7(12)
N12 C12 C22 . . 122.8(7)
N12 C12 H12A . . 118.6
C22 C12 H12A . . 118.6
C12 C22 C32 . . 118.7(7)
C12 C22 H22A . . 120.7
C32 C22 H22A . . 120.7
C52 C42 C32 . . 118.8(7)
C52 C42 H42A . . 120.6
C32 C42 H42A . . 120.6
N12 C52 C42 . . 122.8(7)
N12 C52 H52A . . 118.6
C42 C52 H52A . . 118.6
N22 C62 C72 . . 122.7(7)
N22 C62 H62A . . 118.6
C72 C62 H62A . . 118.6
C62 C72 C82 . . 118.4(7)
C62 C72 H72A . . 120.8
C82 C72 H72A . . 120.8
C102 C92 C82 . . 118.3(6)
C102 C92 H92A . . 120.9
C82 C92 H92A . . 120.9
N22 C102 C92 . . 122.3(7)
N22 C102 H10A . . 118.8
C92 C102 H10A . . 118.8
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Co1 O41 1_455 2.022(14)
Co1 O1W . 2.051(18)
Co1 N12 . 2.171(6)
Co1 O21 . 2.176(16)
Co1 O2W . 2.192(19)
Co1 N22 1_545 2.202(6)
N12 C52 . 1.326(9)
N12 C12 . 1.329(9)
N22 C62 . 1.331(9)
N22 C102 . 1.335(8)
N22 Co1 1_565 2.202(6)
C32 C42 . 1.401(10)
C32 C22 . 1.402(10)
C32 C82 . 1.470(10)
C82 C72 . 1.404(10)
C82 C92 . 1.415(9)
O11 C71 . 1.267(13)
O21 C71 . 1.267(11)
O31 C81 . 1.265(14)
O41 C81 . 1.264(11)
O41 Co1 1_655 2.022(14)
C11 C61 . 1.377(9)
C11 C21 . 1.382(9)
C11 C71 . 1.550(12)
C21 C31 . 1.385(9)
C21 H21A . 0.9300
C31 C41 . 1.384(9)
C31 H31A . 0.9300
C41 C51 . 1.387(9)
C41 H41A . 0.9300
C51 C61 . 1.384(9)
C51 H51A . 0.9300
C61 C81 . 1.547(12)
C12 C22 . 1.389(10)
C12 H12A . 0.9300
C22 H22A . 0.9300
C42 C52 . 1.391(10)
C42 H42A . 0.9300
C52 H52A . 0.9300
C62 C72 . 1.387(10)
C62 H62A . 0.9300
C72 H72A . 0.9300
C92 C102 . 1.391(10)
C92 H92A . 0.9300
C102 H10A . 0.9300
