A new dynamic framework with direct in situ visualisation of breathing under CO2 gas pressure
Sikiti, Phumile; Bezuidenhout, Charl X.; van Heerden, Dewald P.; Barbour, Leonard J.; CrystEngComm 21 (2019) 3415–; doi:10.1039/C9CE00418A

data_7232721
_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         '0.13(C352 H288 Co16 N32 O80)'
_chemical_formula_sum            'C44 H36 Co2 N4 O10'
_chemical_formula_weight         898.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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                 101.808(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.7813(12)
_cell_length_b                   15.7987(7)
_cell_length_c                   23.7492(9)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.149
_cell_measurement_theta_min      2.67
_cell_volume                     10937.7(8)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker SMART CCD 1K area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 1K area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1097
_diffrn_reflns_av_unetI/netI     0.0819
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            135400
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.07
_diffrn_reflns_theta_min         1.97
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    0.655
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_correction_T_min  0.815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1050 before and 0.0792 after correction. The Ratio of minimum to maximum transmission is 0.8532. The \l/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    1.091
_exptl_crystal_description       block
_exptl_crystal_F_000             3696
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.833
_refine_diff_density_min         -1.261
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1081
_refine_ls_number_reflns         21562
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.1456
_refine_ls_R_factor_gt           0.0850
_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/[\s^2^(Fo^2^)+(0.1108P)^2^+51.8478P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2411
_refine_ls_wR_factor_ref         0.2894
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11751
_reflns_number_total             21562
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00418a4.cif
_cod_data_source_block           cob1-dmf
_cod_depositor_comments
'Adding full bibliography for 7232721--7232725.cif.'
_cod_database_code               7232721
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.922
_shelx_estimated_absorpt_t_min   0.815
_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:
 C74(H74A,H74B), C44(H44A,H44B), C22(H22A,H22B), C72(H72A,H72B), C73(H73A,
 H73B), C46(H46A,H46B), C45(H45A,H45B), C42(H42A,H42B), C43(H43A,H43B),
 C47(H47A,H47B), C21(H21A,H21B), C20(H20A,H20B)
2.b Aromatic/amide H refined with riding coordinates:
 C34(H34), C50(H50), C71(H71), C3(H3), C64(H64), C37(H37), C55(H55), C7(H7),
 C81(H81), C84(H84), C49(H49), C12(H12), C35(H35), C77(H77), C59(H59), C32(H32),
  C6(H6), C83(H83), C38(H38), C28(H28), C31(H31), C29(H29), C70(H70), C61(H61),
 C56(H56), C25(H25), C4(H4), C62(H62), C13(H13), C15(H15), C26(H26), C80(H80),
 C51(H51), C58(H58), C52(H52), C67(H67), C78(H78), C87(H87), C86(H86), C41(H41),
  C65(H65), C18(H18), C19(H19), C68(H68), C40(H40), C16(H16), C10(H10), C9(H9)
;
_olex2_submission_special_instructions 'No special instructions were received'