The impact of solid solution composition on kinetics and mechanism of [2 + 2] photodimerization of cinnamic acid derivatives
Pandolfi, Lorenzo; Giunchi, Andrea; Salzillo, Tommaso; Brillante, Aldo; Della Valle, Raffaele G.; Venuti, Elisabetta; Grepioni, Fabrizia; D'Agostino, Simone; CrystEngComm 23 (2021) 1352–1359; doi:10.1039/D0CE01718C

data_7241977
_publ_section_title
;
 The impact of solid solution composition on kinetics and mechanism of [2
 + 2] photodimerization of cinnamic acid derivatives
;
_journal_issue                   6
_journal_name_full               CrystEngComm
_journal_page_first              1352
_journal_page_last               1359
_journal_paper_doi               10.1039/D0CE01718C
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         '0.5(Br Cl), C9 H10 N O2'
_chemical_formula_sum            'C9 H10 Br0.5 Cl0.5 N O2'
_chemical_formula_weight         221.86
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-16 deposited with the CCDC.	2020-12-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.210(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.7177(2)
_cell_length_b                   8.6998(4)
_cell_length_c                   19.4040(9)
_cell_measurement_reflns_used    1305
_cell_measurement_temperature    300
_cell_measurement_theta_max      25.4490
_cell_measurement_theta_min      4.0560
_cell_volume                     964.49(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      300
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1340
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.9982
_diffrn_measured_fraction_theta_max 0.8363
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            3954
_diffrn_reflns_theta_full        25.0000
_diffrn_reflns_theta_max         29.22
_diffrn_reflns_theta_min         3.57
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.295
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97593
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.5278
_exptl_crystal_description       block
_exptl_crystal_F_000             451.9386
_exptl_crystal_recrystallization_method 'slow evaporation of a water solution'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.6237
_refine_diff_density_min         -0.4609
_refine_diff_density_rms         0.1219
_refine_ls_d_res_high            0.7280
_refine_ls_d_res_low             5.7134
_refine_ls_goodness_of_fit_ref   1.0283
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    18
_refine_ls_number_parameters     123
_refine_ls_number_reflns         2187
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0283
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0459P)^2^+0.4866P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1220
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              7
_reflns_limit_h_min              -7
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                1530
_reflns_number_total             2187
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0ce01718c2.cif
_cod_data_source_block           '[1H]Br05Cl05'
_cod_depositor_comments
'Adding full bibliography for 7241976--7241984.cif.'
_cod_database_code               7241977
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Others
 Fixed Sof: Br1(0.5) Cl1(0.5)
 Fixed X: Br1(0.109449) Cl1(0.10409)
 Fixed Y: Br1(0.29206) Cl1(0.285509)
 Fixed Z: Br1(0.776369) Cl1(0.76274)
3.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C3(H3), C2(H2a), C8(H8), C6(H6), C5(H5)
3.b Idealised Me refined as rotating group:
 N1(H1a,H1b,H1c)
3.c Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_olex2_exptl_crystal_mounting_method 'foblin oil'
_olex2_submission_special_instructions 'No special instructions were received'