Structure-switching M<sub>3</sub>L<sub>2</sub> Ir(iii) coordination cages with photo-isomerising azo-aromatic linkers.
Oldknow, Samuel; Martir, Diego Rota; Pritchard, Victoria E.; Blitz, Mark A.; Fishwick, Colin W. G.; Zysman-Colman, Eli; Hardie, Michaele J.; Chemical science 9 (2018) 8150–8159; doi:10.1039/c8sc03499k

data_1549883
_publ_section_title
;
 Structure-switching M<sub>3</sub>L<sub>2</sub> Ir(iii) coordination cages
 with photo-isomerising azo-aromatic linkers.
;
_journal_issue                   42
_journal_name_full               'Chemical science'
_journal_page_first              8150
_journal_page_last               8159
_journal_paper_doi               10.1039/c8sc03499k
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C12 H8 N3 O2, H10 Na O5'
_chemical_formula_sum            'C12 H18 N3 Na O7'
_chemical_formula_weight         339.28
_chemical_name_systematic
;
decaaquodisodium 4-[2-(3-pyridyl)diazenyl]-benzoate 
 
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-03-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2018-04-26 deposited with the CCDC.
2018-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 102.838(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.5197(6)
_cell_length_b                   35.222(3)
_cell_length_c                   7.2310(7)
_cell_measurement_reflns_used    2519
_cell_measurement_temperature    119.99(14)
_cell_measurement_theta_max      30.4590
_cell_measurement_theta_min      3.3460
_cell_volume                     1619.0(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.99(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -31.00   -4.00   0.3000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.7322  -57.0000   30.0000 90

  2 omega  -57.00  -12.00   0.3000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509  -19.0000    0.0000 150

  3 omega   11.00   36.50   0.3000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509  -57.0000  -90.0000 85

  4 omega  -56.00   28.00   0.3000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509  -37.0000 -120.0000 280

  5 omega  -81.00    4.50   0.3000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.7322  -61.0000  131.0315 285
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0371242000
_diffrn_orient_matrix_UB_12      -0.0183018000
_diffrn_orient_matrix_UB_13      0.0321873000
_diffrn_orient_matrix_UB_21      0.0749789000
_diffrn_orient_matrix_UB_22      0.0083890000
_diffrn_orient_matrix_UB_23      0.0750361000
_diffrn_orient_matrix_UB_31      -0.0738323000
_diffrn_orient_matrix_UB_32      -0.0006647000
_diffrn_orient_matrix_UB_33      0.0587060000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_unetI/netI     0.0650
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            11758
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.11
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.136
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.969
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.259
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         4026
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.259
_refine_ls_R_factor_all          0.1114
_refine_ls_R_factor_gt           0.0911
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+2.1733P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1631
_refine_ls_wR_factor_ref         0.1714
_reflns_number_gt                3315
_reflns_number_total             4026
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8sc03499k2.cif
_cod_data_source_block           c
_cod_depositor_comments
'Adding full bibliography for 1549883--1549886.cif.'
_cod_database_code               1549883
_chemical_oxdiff_formula         'C48 H72 N12 Na4 O28'
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11)
;
_olex2_date_sample_data_collection 2015-05-21
_olex2_submission_special_instructions 'No special instructions were received'