Crystalline-state chemiluminescence reactions of two-fluorophore-linked adamantylideneadamantane 1,2-dioxetane isomers accompanied by solid-to-solid phase transitions
Matsuhashi, Chihiro; Oyama, Hironaga; Uekusa, Hidehiro; Sato-Tomita, Ayana; Ichiyanagi, Kouhei; Maki, Shojiro A.; Hirano, Takashi; CrystEngComm  (2022) –; doi:10.1039/D2CE00266C

data_7244773
_publ_section_title
;
 Crystalline-state chemiluminescence reactions of two-fluorophore-linked
 adamantylideneadamantane 1,2-dioxetane isomers accompanied by
 solid-to-solid phase transitions
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00266C
_journal_year                    2022
_chemical_formula_sum            'C68 H56 F6 N2 O12'
_chemical_formula_weight         1207.14
_chemical_properties_physical    Light-sensitive,Light-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2019/2
_audit_update_record
;
2022-04-06 deposited with the CCDC.	2022-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.158(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.409(15)
_cell_length_b                   17.899(6)
_cell_length_c                   12.633(5)
_cell_measurement_reflns_used    43430
_cell_measurement_temperature    95(2)
_cell_measurement_theta_max      22.031
_cell_measurement_theta_min      1.427
_cell_volume                     6302(5)
_computing_cell_refinement       XDS
_computing_data_collection       XDS
_computing_data_reduction        XDS
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      95(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'single-axis ball bearing diffractometer'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.750
_diffrn_reflns_av_R_equivalents  0.0836
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            43430
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        22.031
_diffrn_reflns_theta_max         22.031
_diffrn_reflns_theta_min         1.427
_diffrn_source                   synchrotron
_diffrn_source_type              'KEK PF AR-NW12A'
_exptl_absorpt_coefficient_mu    0.099
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_description       needle
_exptl_crystal_F_000             2512
_exptl_crystal_preparation       Luminescent,Luminescent
_exptl_crystal_size_max          0.254
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.006
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       0.0028(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     796
_refine_ls_number_reflns         6588
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0747
_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^)+(0.1005P)^2^+10.9506P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2014
_refine_ls_wR_factor_ref         0.2230
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4384
_reflns_number_total             6588
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00266c4.cif
_cod_data_source_block           2-127-6_sq
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7244773
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_min   0.975
_shelx_estimated_absorpt_t_max   1.000
_shelx_res_checksum              74717
_shelx_fab_checksum              86014