Structure-function relationships of donor-acceptor Stenhouse adduct photochromic switches.
Mallo, Neil; Foley, Eric D.; Iranmanesh, Hasti; Kennedy, Aaron D. W.; Luis, Ena T.; Ho, Junming; Harper, Jason B.; Beves, Jonathon E.; Chemical science 9 (2018) 8242–8252; doi:10.1039/c8sc03218a

data_1549928
_publ_section_title
;
 Structure-function relationships of donor-acceptor Stenhouse adduct
 photochromic switches.
;
_journal_issue                   43
_journal_name_full               'Chemical science'
_journal_page_first              8242
_journal_page_last               8252
_journal_paper_doi               10.1039/c8sc03218a
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C19 H21 N3 O4, 3.5(H2 O)'
_chemical_formula_sum            'C19 H28 N3 O7.5'
_chemical_formula_weight         418.44
_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_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-04-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_audit_update_record
;
2018-04-24 deposited with the CCDC.
2018-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.957(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.253(2)
_cell_length_b                   15.863(3)
_cell_length_c                   22.909(5)
_cell_measurement_reflns_used    9576
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.877
_cell_measurement_theta_min      1.569
_cell_volume                     4027.8(14)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       '<i>APEX3 </i>(Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker kappa APEXII CCD Diffractometer'
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0729
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            108223
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.877
_diffrn_reflns_theta_min         1.569
_diffrn_source                   'Incoatec I\mS microfocus X-ray source'
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_description       block
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.432
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0.0020(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         9576
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0732
_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^)+(0.0837P)^2^+7.0807P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1872
_refine_ls_wR_factor_ref         0.2083
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6975
_reflns_number_total             9576
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc03218a2.cif
_cod_data_source_block           9b
_cod_depositor_comments
;

2019-02-09
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel

 Adding full bibliography for 1549921--1549929.cif.
;
_cod_original_cell_volume        4027.9(15)
_cod_original_formula_moiety     '2(C19 H21 N3 O4), 7(H2 O)'
_cod_original_formula_sum        'C38 H56 N6 O15'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     836.88
_cod_database_code               1549928
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.972
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Riding coordinates:
 O1A(H1AA,H1AB), O2A(H2AA,H2AB), O3A(H3AA,H3AB), O4A(H4AA,H4AB), O5A(H5AA,
 H5AB), O6A(H6AA,H6AB), O7A(H7AA,H7AB)
2.b Ternary CH refined with riding coordinates:
 C7(H7), C11(H11), C7'(H7'), C11'(H11')
2.c Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C13'(H13C,H13D)
2.d Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C9'(H9'),
 C10'(H10'), C15'(H15'), C16'(H16'), C17'(H17'), C18'(H18'), C19'(H19')
2.e Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C12(H12A,H12B,H12C), C2'(H2'A,H2'B,H2'C),
 C3'(H3'A,H3'B,H3'C), C12'(H12D,H12E,H12F)
;
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_funding_html
;
;