Crystal Melting by Light: X-ray Crystal Structure Analysis of an Azo Crystal Showing Photoinduced Crystal-Melt Transition.
Hoshino, Manabu; Uchida, Emi; Norikane, Yasuo; Azumi, Reiko; Nozawa, Shunsuke; Tomita, Ayana; Sato, Tokushi; Adachi, Shin-Ichi; Koshihara, Shin-Ya; Journal of the American Chemical Society 136 (2014) 9158–9164; doi:10.1021/ja503652c

data_4122014
_publ_section_title
;
 Crystal Melting by Light: X-ray Crystal Structure Analysis of an Azo
 Crystal Showing Photoinduced Crystal-Melt Transition.
;
_journal_issue                   25
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9158
_journal_page_last               9164
_journal_paper_doi               10.1021/ja503652c
_journal_volume                  136
_journal_year                    2014
_chemical_formula_sum            'C74 H116 N4 O4'
_chemical_formula_weight         1125.71
_space_group_IT_number           2
_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
_cell_angle_alpha                111.6890(14)
_cell_angle_beta                 104.6421(10)
_cell_angle_gamma                102.2580(11)
_cell_formula_units_Z            2
_cell_length_a                   12.5100(3)
_cell_length_b                   18.0407(5)
_cell_length_c                   18.8888(6)
_cell_measurement_temperature    293(2)
_cell_volume                     3604.13(19)
_computing_cell_refinement       'Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'marccd software (Doyle, 2006)'
_computing_data_reduction        'Denzo (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2011 (Burla et al., 2011)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.881
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_device_type  'MarCCD 165 with MarDTB'
_diffrn_measurement_method       'phi scan'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_radiation_source         'PF-AR NW14A undulator beamline'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68889
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24662
_diffrn_reflns_theta_full        20.37
_diffrn_reflns_theta_max         20.37
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_T_max  0.98401
_exptl_absorpt_correction_T_min  0.96897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'PLATON-MULABS was used (A.L.Spek, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.037
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.205
_refine_diff_density_min         -0.167
_refine_diff_density_rms         0.028
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     742
_refine_ls_number_reflns         6860
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0763
_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^)+(0.1862P)^2^+0.1083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2256
_refine_ls_wR_factor_ref         0.2500
_reflns_number_gt                5024
_reflns_number_total             6860
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja503652c_si_002.cif
_cod_data_source_block           293K
_cod_depositor_comments
'Adding full bibliography for 4122010--4122014.cif.'
_cod_original_cell_volume        3604.12(17)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4122014