Blue light-promoted photolysis of aryldiazoacetates.
Jurberg, Igor D.; Davies, Huw M. L.; Chemical science 9 (2018) 5112–5118; doi:10.1039/c8sc01165f

data_1549438
_publ_section_title
;
 Blue light-promoted photolysis of aryldiazoacetates.
;
_journal_issue                   22
_journal_name_full               'Chemical science'
_journal_page_first              5112
_journal_page_last               5118
_journal_paper_doi               10.1039/c8sc01165f
_journal_volume                  9
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C15 H16 O2'
_chemical_formula_sum            'C15 H16 O2'
_chemical_formula_weight         228.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2017-11-17
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2017.10.03 svn.r3461 for OlexSys, GUI svn.r5395)
;
_audit_update_record
;
2018-02-14 deposited with the CCDC.
2018-05-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.240(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.6189(2)
_cell_length_b                   8.0477(2)
_cell_length_c                   8.68530(10)
_cell_measurement_reflns_used    6379
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.1380
_cell_measurement_theta_min      5.1950
_cell_volume                     590.88(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 HyPix
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
'List of Runs (angles in degrees, time in seconds):'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1716222000
_diffrn_orient_matrix_UB_12      0.0396937000
_diffrn_orient_matrix_UB_13      0.0805373000
_diffrn_orient_matrix_UB_21      -0.0500601000
_diffrn_orient_matrix_UB_22      0.0018691000
_diffrn_orient_matrix_UB_23      0.1609051000
_diffrn_orient_matrix_UB_31      0.0357931000
_diffrn_orient_matrix_UB_32      -0.1871119000
_diffrn_orient_matrix_UB_33      0.0187110000
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6438
_diffrn_reflns_point_group_measured_fraction_full 0.949
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        67.120
_diffrn_reflns_theta_max         67.120
_diffrn_reflns_theta_min         5.232
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.666
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.253
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_description       block
_exptl_crystal_F_000             244
_exptl_crystal_recrystallization_method
'The material was recrystallised from CHCl3 by slow evaporation'
_exptl_crystal_size_max          0.544
_exptl_crystal_size_mid          0.413
_exptl_crystal_size_min          0.228
_refine_diff_density_max         0.198
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Flack x determined using 861 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.06(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         2010
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0283
_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^)+(0.0477P)^2^+0.0735P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0719
_reflns_Friedel_coverage         0.776
_reflns_Friedel_fraction_full    0.900
_reflns_Friedel_fraction_max     0.900
_reflns_number_gt                1986
_reflns_number_total             2010
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc01165f2.cif
_cod_data_source_block           idj323f2
_cod_depositor_comments          'Adding full bibliography for 1549438.cif.'
_cod_database_code               1549438
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C30  H32  O4  '
_reflns_odcompleteness_completeness 98.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.29
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All H(H,H) groups, All H(H,H,H,H,H,H,H) groups
2. Restrained distances
 C9-H9C \\sim C9-H9A \\sim C9-H9B
 with sigma of 0.002
 H9C-H9A \\sim H9C-H9B \\sim H9B-H9A
 with sigma of 0.004
 C2-H2 \\sim C3-H3
 with sigma of 0.002
 C7-H7B \\sim C7-H7A
 with sigma of 0.002
 C4-H4A \\sim C4-H4B \\sim C7-H7B
 with sigma of 0.002
 H7B-H7A \\sim H4B-H4A
 with sigma of 0.004
 C6-H6 \\sim C5-H5
 with sigma of 0.002
 C15-H15 \\sim C14-H14 \\sim C13-H13 \\sim C12-H12 \\sim C11-H11
 with sigma of 0.002
 H15-H14 \\sim H12-H11
 with sigma of 0.004
 H13-H12 \\sim H14-H13
 with sigma of 0.003
3. Uiso/Uaniso restraints and constraints
Uiso(H9B) = Uiso(H9C) = Uiso(H9A)
Uiso(H2) = Uiso(H3)
Uiso(H7A) = Uiso(H7B)
Uiso(H4A) = Uiso(H7A)
Uiso(H6) = Uiso(H5)
;
_shelx_res_checksum              65778
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a loop with paratone oil'
_olex2_submission_original_sample_id IDJ323F2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.304
_oxdiff_exptl_absorpt_empirical_full_min 0.814