FRET in Orthogonal Stiff Dyads; Diamond-restriction for Frozen Vibrations.
Langhals, Heinz; Dietl, Christian; Dahl, Jeremy E. P.; Carlson, Robert M. K.; Chern, Yaw-Terng; Mayer, Peter; The Journal of organic chemistry  (2020) –; doi:10.1021/acs.joc.0c01184

data_4038669
_publ_section_title
;
 FRET in Orthogonal Stiff Dyads; Diamond-restriction for Frozen
 Vibrations.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.0c01184
_journal_year                    2020
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C18 H20'
_chemical_formula_sum            'C18 H20'
_chemical_formula_weight         236.34
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_block_code                C18H20_pn266_langhals
_audit_creation_date             05-Aug-11
_audit_creation_method           SHELXL-2018/3
_audit_update_record             08-Jan-20
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5493(5)
_cell_length_b                   14.2703(3)
_cell_length_c                   6.6906(2)
_cell_measurement_reflns_used    5185
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.134
_cell_volume                     1293.64(7)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement
;
Sheldrick, G. M. (2008).
<i>Acta Cryst.</i> A<b>64</b>, 112--122.
;
_computing_structure_solution
;
G. M. Sheldrick: A short history of SHELX; Acta Crystallogr., Sect. A: Found.
Crystallogr. 2008, 64, 112-122.
;
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD; rotation images; thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.0531098
_diffrn_orient_matrix_UB_12      -0.0457609
_diffrn_orient_matrix_UB_13      -0.0490180
_diffrn_orient_matrix_UB_21      0.1348242
_diffrn_orient_matrix_UB_22      0.0023103
_diffrn_orient_matrix_UB_23      0.0301665
_diffrn_orient_matrix_UB_31      -0.0366209
_diffrn_orient_matrix_UB_32      -0.0578595
_diffrn_orient_matrix_UB_33      0.0399727
_diffrn_radiation_collimation    0.20
_diffrn_radiation_monochromator  'MONTEL, graded multilayered X-ray optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            9369
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.478
_diffrn_reflns_theta_min         3.329
_diffrn_source                   'rotating anode'
_diffrn_source_current           55.00
_diffrn_source_power             3.025
_diffrn_source_type              'FR 591 generator'
_diffrn_source_voltage           55.00
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_description       rod
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.204
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 1062 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -1.7(10)
_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     163
_refine_ls_number_reflns         2862
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0479P)^2^+0.1909P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0933
_refine_ls_wR_factor_ref         0.0974
_reflns_Friedel_coverage         0.783
_reflns_Friedel_fraction_full    0.974
_reflns_Friedel_fraction_max     0.924
_reflns_number_gt                2582
_reflns_number_total             2862
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo0c01184_si_002.cif
_cod_data_source_block           pn266
_cod_database_code               4038669
_shelx_estimated_absorpt_t_min   0.982
_shelx_estimated_absorpt_t_max   0.993
_shelx_res_checksum              95193
_shelx_hkl_checksum              11880