#------------------------------------------------------------------------------
#$Date: 2017-04-20 04:44:53 +0300 (Thu, 20 Apr 2017) $
#$Revision: 195605 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/57/1545770.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_1545770
loop_
_publ_author_name
'Gonzalez, Miguel'
'Mason, Jarad'
'Bloch, Eric D.'
'Teat, Simon'
'Gagnon, Kevin J.'
'Morrison, Gregory Y.'
'Queen, Wendy Lee'
'Long, Jeffrey R.'
_publ_section_title
;
 Structural characterization of framework--gas interactions in the
 metal--organic framework Co2(dobdc) by in situ single-crystal X-ray
 diffraction
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC00449D
_journal_year                    2017
_chemical_formula_moiety         '(Co2 C8 H2 O6) 1.19(C O)'
_chemical_formula_sum            'C9.19 H2 Co2 O7.19'
_chemical_formula_weight         345.19
_chemical_name_common            Co2(dobdc)(CO)1.19
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-06-01
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-01-28 deposited with the CCDC.
2017-04-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   25.853(3)
_cell_length_b                   25.853(3)
_cell_length_c                   6.8494(7)
_cell_measurement_reflns_used    8223
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.355
_cell_measurement_theta_min      3.392
_cell_volume                     3964.7(8)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω/θ scans'
_diffrn_radiation_monochromator  'channel-cut Si(111) crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0844
_diffrn_reflns_av_unetI/netI     0.0654
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            24665
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         34.715
_diffrn_reflns_theta_min         3.391
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.407
_exptl_absorpt_correction_T_max  0.910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1437 before and 0.0868 after correction.
 The Ratio of minimum to maximum transmission not present.
 The λ/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1405 before and 0.0840 after correction.
 The Ratio of minimum to maximum transmission is 0.74.
 The λ/2 correction factor is Not present

Final HKLF 4 output contains 24665 reflections, Rint = 0.0844
 (12621 with I > 3sig(I), Rint = 0.0747)
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1518
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         2885
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0302P)²+2.6904P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1032
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2437
_reflns_number_total             2885
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7sc00449d2.cif
_cod_data_source_block           Co2dobdc-COB
_cod_original_cell_volume        3964.6(9)
_cod_database_code               1545770
_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   0.910
_shelx_estimated_absorpt_t_min   0.699
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5681(16) 0.4319(16)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Uiso/Uaniso restraints and constraints
C5 \\sim O4: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 O4, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C5(0.59) O4(0.59)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Co1 Co 0.96921(2) 0.35229(2) 0.14382(4) 0.02214(10) Uani 1 1 d . . .
O2 O 1.03778(7) 0.34128(8) 0.0262(2) 0.0275(3) Uani 1 1 d . . .
O1 O 1.02161(8) 0.41429(7) 0.3379(2) 0.0252(3) Uani 1 1 d . . .
O3 O 0.96802(9) 0.40525(8) -0.0704(2) 0.0308(4) Uani 1 1 d . . .
C2 C 1.12612(10) 0.33960(11) -0.0463(3) 0.0245(4) Uani 1 1 d . . .
C3 C 1.18100(10) 0.34957(11) 0.0249(3) 0.0276(4) Uani 1 1 d . . .
H3 H 1.1907 0.3609 0.1578 0.033 Uiso 1 1 calc R . .
C1 C 1.11145(10) 0.32291(10) -0.2439(3) 0.0234(4) Uani 1 1 d . . .
C4 C 1.08722(9) 0.34921(10) 0.0915(3) 0.0234(4) Uani 1 1 d . . .
C5 C 0.8887(3) 0.3510(3) 0.2608(10) 0.0624(17) Uani 0.59 1 d . U P
O4 O 0.8501(6) 0.3513(9) 0.306(2) 0.294(8) Uani 0.59 1 d . U P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 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'
Co Co 0.3550 1.1300 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0140 0.0070 '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 O2 82.453(19) 6_665 .
O2 Co1 C5 172.3(2) . .
O2 Co1 C5 94.25(19) 6_665 .
O1 Co1 O2 81.78(6) 8_644 6_665
O1 Co1 O2 81.06(7) 8_644 .
O1 Co1 O2 94.85(6) . .
O1 Co1 O2 81.47(6) . 6_665
O1 Co1 O1 163.14(7) . 8_644
O1 Co1 O3 100.00(7) . .
O1 Co1 O3 96.72(7) 8_644 .
O1 Co1 C5 91.6(2) 8_644 .
O1 Co1 C5 91.53(19) . .
O3 Co1 O2 96.54(7) . .
O3 Co1 O2 178.30(7) . 6_665
O3 Co1 C5 86.59(19) . .
Co1 O2 Co1 91.68(6) 8_644 .
C4 O2 Co1 134.04(14) . .
C4 O2 Co1 130.87(14) . 8_644
Co1 O1 Co1 96.69(6) . 6_665
C1 O1 Co1 125.76(12) 8_645 6_665
C1 O1 Co1 125.85(14) 8_645 .
C4 O3 Co1 123.89(14) 8_644 .
C3 C2 C1 118.91(19) . .
C3 C2 C4 117.17(18) . .
C1 C2 C4 123.89(19) . .
C2 C3 H3 118.5 . .
C1 C3 C2 122.91(19) 16_754 .
C1 C3 H3 118.5 16_754 .
O1 C1 C2 124.09(18) 6_664 .
O1 C1 C3 117.72(18) 6_664 16_754
C3 C1 C2 118.18(19) 16_754 .
O2 C4 C2 117.35(18) . .
O3 C4 O2 122.47(19) 6_665 .
O3 C4 C2 120.17(19) 6_665 .
O4 C5 Co1 175.7(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O2 2.0922(16) .
Co1 O2 2.0908(16) 6_665
Co1 O1 2.0161(15) 8_644
Co1 O1 2.0001(15) .
Co1 O3 2.0178(16) .
Co1 C5 2.215(6) .
O2 Co1 2.0909(16) 8_644
O2 C4 1.270(2) .
O1 Co1 2.0160(15) 6_665
O1 C1 1.358(2) 8_645
O3 C4 1.248(2) 8_644
C2 C3 1.397(3) .
C2 C1 1.414(3) .
C2 C4 1.488(3) .
C3 H3 0.9500 .
C3 C1 1.383(3) 16_754
C1 O1 1.359(2) 6_664
C1 C3 1.383(3) 16_754
C4 O3 1.248(2) 6_665
C5 O4 1.046(11) .
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_1
_geom_torsion_site_symmetry_4
Co1 O2 C4 O3 2.8(4) . 6_665
Co1 O2 C4 O3 -150.18(18) 8_644 6_665
Co1 O2 C4 C2 -176.15(15) . .
Co1 O2 C4 C2 30.9(3) 8_644 .
C3 C2 C1 O1 179.6(2) . 6_664
C3 C2 C1 C3 0.1(4) . 16_754
C3 C2 C4 O2 178.7(2) . .
C3 C2 C4 O3 -0.2(3) . 6_665
C1 C2 C3 C1 -0.1(4) . 16_754
C1 C2 C4 O2 0.7(3) . .
C1 C2 C4 O3 -178.3(2) . 6_665
C4 C2 C3 C1 -178.3(2) . 16_754
C4 C2 C1 O1 -2.4(4) . 6_664
C4 C2 C1 C3 178.1(2) . 16_754
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.5681(16)
2 0.4319(16)
