Cavity-Directed Chromism of Phthalein Dyes.
Takezawa, Hiroki; Akiba, Shouta; Murase, Takashi; Fujita, Makoto; Journal of the American Chemical Society 137 (2015) 7043–7046; doi:10.1021/jacs.5b03618

data_4123762
_publ_contact_author             'Makoto Fujita'
_publ_section_title
;
 Cavity-Directed Chromism of Phthalein Dyes.
;
_journal_issue                   22
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7043
_journal_page_last               7046
_journal_paper_doi               10.1021/jacs.5b03618
_journal_volume                  137
_journal_year                    2015
_chemical_formula_sum            'C148 H172 N41.3 O73.1 Pd6'
_chemical_formula_weight         4337.46
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.477(4)
_cell_length_b                   36.360(4)
_cell_length_c                   20.252(2)
_cell_measurement_reflns_used    9833
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      24.20
_cell_measurement_theta_min      2.17
_cell_volume                     24651(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            215458
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        24.237
_diffrn_reflns_theta_max         24.237
_diffrn_reflns_theta_min         1.275
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.506
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.7057
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             8840
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.635
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.152
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.47(4)
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2634
_refine_ls_number_reflns         39429
_refine_ls_number_restraints     381
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0906
_refine_ls_R_factor_gt           0.0740
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1577P)^2^+20.5079P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2011
_refine_ls_wR_factor_ref         0.2217
_reflns_Friedel_coverage         0.939
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                32717
_reflns_number_total             39429
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b03618_si_002.cif
_cod_data_source_block           pna21
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 4123762.cif.
;
_cod_original_formula_sum        'C148 H172 N41.30 O73.10 Pd6'
_cod_database_code               4123762
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.915
_shelx_estimated_absorpt_t_max   0.990
_shelx_res_checksum              4779
_shelx_hkl_checksum              32200