Synthesis of Sterically Fixed Phytochrome Chromophore Derivatives Bearing a 15 E- Fixed or 15 E- Anti- Fixed CD-Ring Component.
Soeta, Takahiro; Ohashi, Nobuhiko; Kobayashi, Toshiharu; Sakata, Yoko; Suga, Takuya; Ukaji, Yutaka; The Journal of organic chemistry 83 (2018) 10743–10748; doi:10.1021/acs.joc.8b01252

data_4035653
_publ_section_title
;
 Synthesis of Sterically Fixed Phytochrome Chromophore Derivatives Bearing
 a 15 E- Fixed or 15 E- Anti- Fixed CD-Ring Component.
;
_journal_issue                   18
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              10743
_journal_page_last               10748
_journal_paper_doi               10.1021/acs.joc.8b01252
_journal_volume                  83
_journal_year                    2018
_chemical_formula_moiety         'C28 H39 Cl N2 O5'
_chemical_formula_sum            'C28 H39 Cl N2 O5'
_chemical_formula_weight         519.06
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                98.0511(12)
_cell_angle_beta                 102.9639(14)
_cell_angle_gamma                93.8281(14)
_cell_formula_units_Z            2
_cell_length_a                   9.4899(5)
_cell_length_b                   10.4443(5)
_cell_length_c                   14.7373(7)
_cell_measurement_reflns_used    18030
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      72.452
_cell_measurement_theta_min      3.117
_cell_volume                     1402.12(12)
_computing_cell_refinement       'SAINT V8.37A/APEX3 (Bruker AXS Inc., 2015)'
_computing_data_collection       'Bruker Instrument Service V4.2.9 '
_computing_data_reduction        'SAINT V8.37A/APEX3 (Bruker AXS Inc., 2015)'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  ORTEP-3
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18030
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.452
_diffrn_reflns_theta_min         3.117
_diffrn_source                   'fine-focus rotating anode'
_exptl_absorpt_coefficient_mu    1.519
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/5 (Sheldrick, 1996 / Bruker AXS)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.050
_exptl_transmission_factor_max   0.7536
_exptl_transmission_factor_min   0.6635
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         5417
_refine_ls_number_restraints     254
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0496
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0781P)^2^+0.6432P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1374
_refine_ls_wR_factor_ref         0.1387
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5153
_reflns_number_total             5417
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo8b01252_si_003.cif
_cod_data_source_block           soeta006_NO5-99
_cod_database_code               4035653
_shelx_estimated_absorpt_t_min   0.804
_shelx_estimated_absorpt_t_max   0.928
_shelxl_version_number           2014-3
_shelx_res_checksum              4636
_shelx_hkl_checksum              86729