#------------------------------------------------------------------------------
#$Date: 2019-11-07 21:21:57 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223489 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/27/7232724.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_7232724
loop_
_publ_author_name
'Sikiti, Phumile'
'Bezuidenhout, Charl X.'
'van Heerden, Dewald P.'
'Barbour, Leonard J.'
_publ_section_title
;
 A new dynamic framework with direct in situ visualisation of breathing
 under CO2 gas pressure
;
_journal_issue                   22
_journal_name_full               CrystEngComm
_journal_page_first              3415
_journal_paper_doi               10.1039/C9CE00418A
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         '0.25(C176 H144 Co8 N16 O40)'
_chemical_formula_sum            'C44 H36 Co2 N4 O10'
_chemical_formula_weight         898.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-03-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-12 deposited with the CCDC.    2019-05-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.360(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.7632(11)
_cell_length_b                   9.8043(5)
_cell_length_c                   20.3897(10)
_cell_measurement_reflns_used    9967
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.07
_cell_measurement_theta_min      2.26
_cell_volume                     4640.3(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      298.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1010
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            53242
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.092
_diffrn_reflns_theta_min         2.255
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.772
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0961 before and 0.0679 after correction. The Ratio of minimum to maximum transmission is 0.9255. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            'clear bluish blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_description       block
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.268
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4122
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0431
_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)+(0.0349P)²+5.5825P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0996
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2754
_reflns_number_total             4122
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9ce00418a4.cif
_cod_data_source_block           10bar
_cod_depositor_comments
'Adding full bibliography for 7232721--7232725.cif.'
_cod_database_code               7232724
_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   0.935
_shelx_estimated_absorpt_t_min   0.820
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B), C20(H20A,H20B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C3(H3), C16(H16), C19(H19), C15(H15), C4(H4), C18(H18), C13(H13),
 C6(H6), C9(H9), C10(H10), C12(H12)
;
_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'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
Co1 Co 0.04752(2) 0.08217(4) 0.01953(2) 0.04673(15) Uani 1 1 d .
O1 O 0.08556(10) -0.0727(2) 0.07782(12) 0.0647(7) Uani 1 1 d .
N2 N 0.24875(11) 0.6055(3) 0.00662(16) 0.0600(8) Uani 1 1 d .
N1 N 0.11712(12) 0.2106(2) 0.02766(15) 0.0494(7) Uani 1 1 d .
O3 O 0.16391(11) -0.6225(3) 0.23633(16) 0.0934(10) Uani 1 1 d .
C1 C 0.05812(16) -0.1840(3) 0.07706(18) 0.0532(9) Uani 1 1 d .
C2 C 0.08772(15) -0.2982(3) 0.11923(18) 0.0533(9) Uani 1 1 d .
C21 C 0.30061(14) 0.6771(3) -0.0021(2) 0.0720(12) Uani 1 1 d .
H21A H 0.322643 0.619192 -0.025900 0.086 Uiso 1 1 calc R
H21B H 0.324547 0.698871 0.041435 0.086 Uiso 1 1 calc R
C7 C 0.13731(17) -0.2794(4) 0.1669(2) 0.0695(11) Uani 1 1 d .
H7 H 0.154247 -0.193548 0.172724 0.083 Uiso 1 1 calc R
C3 C 0.06412(15) -0.4283(4) 0.10947(19) 0.0622(9) Uani 1 1 d .
H3 H 0.030968 -0.442510 0.076513 0.075 Uiso 1 1 calc R
C16 C 0.16678(16) 0.3868(4) -0.0171(2) 0.0716(11) Uani 1 1 d .
H16 H 0.167424 0.447159 -0.052096 0.086 Uiso 1 1 calc R
C19 C 0.16064(16) 0.2090(4) 0.0802(2) 0.0655(10) Uani 1 1 d .
H19 H 0.159326 0.147215 0.114478 0.079 Uiso 1 1 calc R
C17 C 0.21128(14) 0.3853(3) 0.0377(2) 0.0591(10) Uani 1 1 d .
C8 C 0.12944(16) -0.6874(4) 0.2747(2) 0.0738(12) Uani 1 1 d .
C5 C 0.13769(18) -0.5147(4) 0.1966(2) 0.0729(12) Uani 1 1 d .
C22 C 0.21625(16) 0.6938(3) 0.0412(2) 0.0711(12) Uani 1 1 d .
H22A H 0.239254 0.716239 0.085206 0.085 Uiso 1 1 calc R
H22B H 0.181866 0.646823 0.047504 0.085 Uiso 1 1 calc R
C15 C 0.12054(15) 0.2986(4) -0.0207(2) 0.0645(10) Uani 1 1 d .
H15 H 0.090763 0.301245 -0.058649 0.077 Uiso 1 1 calc R
C4 C 0.08920(17) -0.5360(4) 0.1480(2) 0.0727(12) Uani 1 1 d .
H4 H 0.073290 -0.622873 0.140942 0.087 Uiso 1 1 calc R
C20 C 0.26277(15) 0.4780(4) 0.0430(2) 0.0768(12) Uani 1 1 d .
H20A H 0.278419 0.498057 0.089912 0.092 Uiso 1 1 calc R
H20B H 0.292297 0.430883 0.025422 0.092 Uiso 1 1 calc R
C18 C 0.20775(16) 0.2933(4) 0.0873(2) 0.0712(11) Uani 1 1 d .
H18 H 0.237111 0.287974 0.125514 0.085 Uiso 1 1 calc R
C13 C 0.13894(17) -0.8231(4) 0.2868(2) 0.0785(12) Uani 1 1 d .
H13 H 0.165680 -0.869816 0.268001 0.094 Uiso 1 1 calc R
C6 C 0.16246(17) -0.3872(4) 0.2063(2) 0.0778(12) Uani 1 1 d .
H6 H 0.195772 -0.373695 0.239122 0.093 Uiso 1 1 calc R
C9 C 0.08994(19) -0.6182(4) 0.3014(2) 0.0912(15) Uani 1 1 d .
H9 H 0.084042 -0.525514 0.293096 0.109 Uiso 1 1 calc R
O2 O 0.00828(10) -0.2052(2) 0.04448(13) 0.0656(7) Uani 1 1 d .
C11 C 0.06798(14) -0.8225(3) 0.35474(18) 0.0548(9) Uani 1 1 d .
C10 C 0.05900(17) -0.6860(4) 0.3407(2) 0.0802(13) Uani 1 1 d .
H10 H 0.031499 -0.638998 0.358143 0.096 Uiso 1 1 calc R
C12 C 0.10849(16) -0.8898(4) 0.32720(19) 0.0713(11) Uani 1 1 d .
H12 H 0.115250 -0.982094 0.336191 0.086 Uiso 1 1 calc R
C14 C 0.03765(15) -0.8911(3) 0.40238(18) 0.0564(9) Uani 1 1 d .
O4 O 0.06303(10) -0.9897(2) 0.43545(12) 0.0640(7) Uani 1 1 d .
O5 O -0.01033(10) -0.8442(2) 0.40791(12) 0.0642(7) 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'
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
O1 Co1 Co1 88.08(7) . 5
O1 Co1 N1 99.32(10) . .
O1 Co1 O2 165.39(9) . 5
O1 Co1 O4 91.25(10) . 6_545
N1 Co1 Co1 168.09(9) . 5
O2 Co1 Co1 77.33(7) 5 5
O2 Co1 N1 95.20(10) 5 .
O2 Co1 O4 86.28(10) 5 6_545
O4 Co1 Co1 77.37(7) 6_545 5
O4 Co1 N1 93.04(10) 6_545 .
O5 Co1 Co1 87.73(7) 2_565 5
O5 Co1 O1 92.78(10) 2_565 .
O5 Co1 N1 101.13(10) 2_565 .
O5 Co1 O2 86.03(10) 2_565 5
O5 Co1 O4 164.42(9) 2_565 6_545
C1 O1 Co1 118.4(2) . .
C22 N2 C21 108.9(3) . .
C22 N2 C20 110.8(3) . .
C20 N2 C21 111.6(3) . .
C19 N1 Co1 122.3(2) . .
C19 N1 C15 116.7(3) . .
C15 N1 Co1 121.0(2) . .
C5 O3 C8 115.3(3) . .
O1 C1 C2 117.4(3) . .
O2 C1 O1 125.3(3) . .
O2 C1 C2 117.3(3) . .
C7 C2 C1 122.4(3) . .
C7 C2 C3 118.9(3) . .
C3 C2 C1 118.7(3) . .
N2 C21 C22 109.5(3) . 7_565
C2 C7 C6 120.6(4) . .
C4 C3 C2 120.8(4) . .
C17 C16 C15 120.2(4) . .
N1 C19 C18 123.8(3) . .
C16 C17 C20 121.8(3) . .
C16 C17 C18 116.9(3) . .
C18 C17 C20 121.4(4) . .
C13 C8 O3 116.8(3) . .
C9 C8 O3 122.2(3) . .
C9 C8 C13 120.9(3) . .
C4 C5 O3 120.6(4) . .
C4 C5 C6 120.7(4) . .
C6 C5 O3 118.7(4) . .
N2 C22 C21 110.8(3) . 7_565
N1 C15 C16 122.6(4) . .
C5 C4 C3 119.5(4) . .
N2 C20 C17 112.8(3) . .
C17 C18 C19 119.7(4) . .
C8 C13 C12 119.1(4) . .
C5 C6 C7 119.4(4) . .
C8 C9 C10 119.7(4) . .
C1 O2 Co1 130.9(2) . 5
C10 C11 C12 118.1(3) . .
C10 C11 C14 120.0(3) . .
C12 C11 C14 121.7(3) . .
C9 C10 C11 121.0(4) . .
C13 C12 C11 121.2(3) . .
O4 C14 C11 117.0(3) . .
O4 C14 O5 125.0(3) . .
O5 C14 C11 117.9(3) . .
C14 O4 Co1 129.8(2) . 6_546
C14 O5 Co1 119.0(2) . 2_545
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 Co1 2.7497(8) 5
Co1 O1 2.018(2) .
Co1 N1 2.057(2) .
Co1 O2 2.044(2) 5
Co1 O4 2.041(2) 6_545
Co1 O5 2.012(2) 2_565
O1 C1 1.270(4) .
N2 C21 1.462(4) .
N2 C22 1.442(4) .
N2 C20 1.455(4) .
N1 C19 1.321(4) .
N1 C15 1.326(4) .
O3 C8 1.400(4) .
O3 C5 1.394(4) .
C1 C2 1.492(5) .
C1 O2 1.245(4) .
C2 C7 1.370(5) .
C2 C3 1.391(4) .
C21 C22 1.504(5) 7_565
C7 C6 1.384(5) .
C3 C4 1.374(5) .
C16 C17 1.364(5) .
C16 C15 1.388(4) .
C19 C18 1.374(4) .
C17 C20 1.510(4) .
C17 C18 1.371(5) .
C8 C13 1.363(5) .
C8 C9 1.363(5) .
C5 C4 1.366(5) .
C5 C6 1.378(5) .
C13 C12 1.373(5) .
C9 C10 1.369(5) .
C11 C10 1.376(5) .
C11 C12 1.382(4) .
C11 C14 1.489(4) .
C14 O4 1.256(4) .
C14 O5 1.257(4) .
