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_1549886
_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_sum            'C60 H30 N9 O9'
_chemical_formula_weight         1020.93
_chemical_name_systematic
; 
2,7,12-trimethoxy-3,8,13-tris(4,3?-pyridyl-azophenylcarboxy)-10,15-dihydro-5H-tribenzo[a,d,g]cyclononene 
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2018-04-26 deposited with the CCDC.
2018-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                71.898(8)
_cell_angle_beta                 88.532(6)
_cell_angle_gamma                89.954(5)
_cell_formula_units_Z            4
_cell_length_a                   9.6864(5)
_cell_length_b                   29.786(2)
_cell_length_c                   34.468(4)
_cell_measurement_reflns_used    4571
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      20.1510
_cell_measurement_theta_min      1.5460
_cell_volume                     9449.1(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega -145.00   25.00   1.0000    0.0964
omega____ theta____ kappa____ phi______ frames
    -       30.0000    0.0000    0.0000 170

  2 omega -145.00   25.00   1.0000    0.0964
omega____ theta____ kappa____ phi______ frames
    -       30.0000    0.0000  120.0000 170

  3 omega -145.00   25.00   1.0000    0.0964
omega____ theta____ kappa____ phi______ frames
    -       30.0000    0.0000  240.0000 170

  4 phi      0.00  180.00   1.0000    0.0964
omega____ theta____ kappa____ phi______ frames
   0.0000    0.0000    0.0000     -     180
;
_diffrn_measurement_device_type  'CCD plate'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.1479
_diffrn_reflns_av_sigmaI/netI    0.1639
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            60957
_diffrn_reflns_theta_full        20.00
_diffrn_reflns_theta_max         20.00
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.050
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28437
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    0.718
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2100
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.711
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         19323
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.717
_refine_ls_R_factor_all          0.3324
_refine_ls_R_factor_gt           0.2253
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4559
_refine_ls_wR_factor_ref         0.4885
_reflns_number_gt                5761
_reflns_number_total             19323
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8sc03499k2.cif
_cod_data_source_block           c_CCDC1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 1549883--1549886.cif.
;
_cod_original_cell_volume        9448.9(13)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1549886
_platon_squeeze_void_probe_radius 1.20