#------------------------------------------------------------------------------
#$Date: 2017-09-06 05:25:33 +0300 (Wed, 06 Sep 2017) $
#$Revision: 200194 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/41/7044114.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_7044114
loop_
_publ_author_name
'Gunatilleke, Wilarachchige D. C. Bhagya'
'Wei, Kaya'
'Niu, Zheng'
'Wojtas, Lukasz'
'Ma, Shengqian'
'Nolas, George S.'
_publ_section_title
;
 Thermal Conductivity of Perovskite-type Metal-Organic Framework Crystal
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02927F
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C3 H3 Co O6, H5 N2'
_chemical_formula_sum            'C3 H8 Co N2 O6'
_chemical_formula_weight         227.04
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-06-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-07-30 deposited with the CCDC.
2017-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6592(3)
_cell_length_b                   7.7641(2)
_cell_length_c                   11.5528(4)
_cell_measurement_reflns_used    4327
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      76.76
_cell_measurement_theta_min      7.66
_cell_volume                     776.71(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      298.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0993
_diffrn_reflns_av_unetI/netI     0.0595
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11359
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         77.117
_diffrn_reflns_theta_min         3.826
_diffrn_source                   'INCOATEC Imus micro-focus source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.430
_exptl_absorpt_correction_T_max  0.3474
_exptl_absorpt_correction_T_min  0.1539
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1554 before and 0.0938 after correction.
The Ratio of minimum to maximum transmission is 0.4430.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_description       block
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.114
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.058
_refine_diff_density_max         0.565
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
;
 Flack x determined using 508 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.001(7)
_refine_ls_extinction_coef       0.0052(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         1620
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0388
_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)+(0.0420P)²+0.3545P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0951
_reflns_Friedel_coverage         0.905
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                1282
_reflns_number_total             1620
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt02927f2.cif
_cod_data_source_block           co_formate_298k
_cod_database_code               7044114
_shelx_shelxl_version_number     2016/6
_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.
;
_shelx_estimated_absorpt_t_max   0.431
_shelx_estimated_absorpt_t_min   0.241
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.524(14)
 0.476(14)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All N(H) groups, All N(H,H,H) groups
3. Restrained distances
 N11-H11B = N11-H11A
 0.91 with sigma of 0.02
 H11A-H11B
 1.51 with sigma of 0.04
 H11B-N12 = N12-H11A
 1.92 with sigma of 0.04
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C9(H9)
4.b Idealised Me refined as rotating group:
 N12(H12A,H12B,H12C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
Co1 Co 0.47612(8) 0.49995(18) 0.5066(2) 0.0164(3) Uani 1 1 d .
O2 O 0.3796(5) 0.7276(6) 0.4409(4) 0.0258(10) Uani 1 1 d .
C3 C 0.2486(9) 0.7779(10) 0.4695(7) 0.0288(16) Uani 1 1 d .
H3 H 0.188811 0.703480 0.513888 0.035 Uiso 1 1 calc R
O4 O 0.1910(5) 0.9195(6) 0.4435(5) 0.0270(10) Uani 1 1 d .
O5 O 0.4499(6) 0.3617(8) 0.3519(4) 0.0273(12) Uani 1 1 d .
C6 C 0.4729(8) 0.4386(8) 0.2570(9) 0.0247(16) Uani 1 1 d .
H6 H 0.480664 0.558052 0.258403 0.030 Uiso 1 1 calc R
O7 O 0.4858(6) 0.3652(8) 0.1627(5) 0.0283(12) Uani 1 1 d .
O8 O 0.2637(5) 0.4157(6) 0.5773(5) 0.0254(10) Uani 1 1 d .
C9 C 0.1937(8) 0.2885(9) 0.5361(6) 0.0274(17) Uani 1 1 d .
H9 H 0.235041 0.237155 0.470336 0.033 Uiso 1 1 calc R
O10 O 0.0734(5) 0.2258(6) 0.5765(5) 0.0279(11) Uani 1 1 d .
N11 N 0.5880(12) -0.0089(11) 0.2280(10) 0.054(3) Uani 1 1 d D
H11A H 0.605(9) 0.090(7) 0.186(8) 0.082 Uiso 1 1 d DR
H11B H 0.584(9) -0.106(8) 0.183(8) 0.09(5) Uiso 1 1 d D
N12 N 0.4355(10) 0.0087(8) 0.2737(8) 0.0346(19) Uani 1 1 d D
H12A H 0.366927 -0.018724 0.219363 0.052 Uiso 1 1 calc GR
H12B H 0.420450 0.117033 0.296128 0.052 Uiso 1 1 calc GR
H12C H 0.424223 -0.061387 0.334080 0.052 Uiso 1 1 calc GR
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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
O2 Co1 O7 87.3(2) . 2_665
O2 Co1 O8 93.09(19) . .
O2 Co1 O10 178.6(3) . 4
O4 Co1 O2 88.6(2) 4_565 .
O4 Co1 O5 87.3(2) 4_565 .
O4 Co1 O7 90.6(2) 4_565 2_665
O4 Co1 O8 177.5(3) 4_565 .
O4 Co1 O10 91.54(19) 4_565 4
O5 Co1 O2 94.6(2) . .
O5 Co1 O7 177.1(3) . 2_665
O5 Co1 O8 94.4(2) . .
O5 Co1 O10 86.8(2) . 4
O7 Co1 O8 87.7(2) 2_665 .
O10 Co1 O7 91.3(2) 4 2_665
O10 Co1 O8 86.7(2) 4 .
C3 O2 Co1 122.1(5) . .
O2 C3 H3 117.3 . .
O4 C3 O2 125.4(8) . .
O4 C3 H3 117.3 . .
C3 O4 Co1 122.5(5) . 4_465
C6 O5 Co1 118.7(5) . .
O5 C6 H6 117.9 . .
O7 C6 O5 124.2(6) . .
O7 C6 H6 117.9 . .
C6 O7 Co1 122.6(5) . 2_664
C9 O8 Co1 121.2(5) . .
O8 C9 H9 117.5 . .
O10 C9 O8 125.0(7) . .
O10 C9 H9 117.5 . .
C9 O10 Co1 121.2(5) . 4_455
H11A N11 H11B 113(6) . .
N12 N11 H11A 106(5) . .
N12 N11 H11B 105(5) . .
N11 N12 H12A 109.5 . .
N11 N12 H12B 109.5 . .
N11 N12 H12C 109.5 . .
H12A N12 H12B 109.5 . .
H12A N12 H12C 109.5 . .
H12B N12 H12C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O2 2.098(5) .
Co1 O4 2.094(5) 4_565
Co1 O5 2.098(6) .
Co1 O7 2.110(6) 2_665
Co1 O8 2.116(5) .
Co1 O10 2.105(5) 4
O2 C3 1.245(9) .
C3 H3 0.9300 .
C3 O4 1.244(9) .
O5 C6 1.264(11) .
C6 H6 0.9300 .
C6 O7 1.235(12) .
O8 C9 1.253(8) .
C9 H9 0.9300 .
C9 O10 1.241(8) .
N11 H11A 0.92(3) .
N11 H11B 0.92(3) .
N11 N12 1.428(11) .
N12 H12A 0.8900 .
N12 H12B 0.8900 .
N12 H12C 0.8900 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N11 H11A O7 0.92(3) 2.39(6) 3.128(11) 137(6) .
N11 H11B O10 0.92(3) 2.25(6) 3.043(11) 144(7) 3_544
N12 H12A O8 0.89 2.06 2.940(10) 171.4 3_544
N12 H12B O5 0.89 2.02 2.888(9) 164.2 .
N12 H12C O2 0.89 2.09 2.954(10) 164.5 1_545
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_4
Co1 O2 C3 O4 172.1(6) .
Co1 O5 C6 O7 167.6(6) .
Co1 O8 C9 O10 175.9(6) .
O2 C3 O4 Co1 -175.1(6) 4_465
O5 C6 O7 Co1 179.9(5) 2_664
O8 C9 O10 Co1 -175.3(6) 4_455
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.524(14)
2 0.476(14)
