Efficient synthesis of 5-oxatruxene and the unusual influence of oxygen heteroatom on its physico-chemical properties
Górski, Krzysztof; Mech-Piskorz, Justyna; Noworyta, Krzysztof; Leśniewska, Barbara; Pietraszkiewicz, Marek; New Journal of Chemistry 42 (2018) 5844–; doi:10.1039/C7NJ04729K

data_7057075
_publ_section_title
;
 Efficient synthesis of 5-oxatruxene and the unusual influence of oxygen
 heteroatom on its physico-chemical properties
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              5844
_journal_paper_doi               10.1039/C7NJ04729K
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         '3(C39 H42)'
_chemical_formula_sum            'C39 H42'
_chemical_formula_weight         510.73
_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'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-01-12 deposited with the CCDC.
2018-02-28 downloaded from the CCDC.
;
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            12
_cell_length_a                   14.1319(4)
_cell_length_b                   12.1283(4)
_cell_length_c                   52.278(3)
_cell_measurement_reflns_used    9011
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      71.4830
_cell_measurement_theta_min      4.4310
_cell_volume                     8960.2(6)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector_area_resol_mean 16.2974
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       -64
_diffrn_reflns_number            29251
_diffrn_reflns_point_group_measured_fraction_full 0.791
_diffrn_reflns_point_group_measured_fraction_max 0.774
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.506
_diffrn_reflns_theta_min         3.740
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.473
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61176
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_description       plate
_exptl_crystal_F_000             3312
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
;
 Flack x determined using 3629 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.6(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1340
_refine_ls_number_reflns         13515
_refine_ls_number_restraints     1170
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0622
_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^)+(0.1068P)^2^+4.4798P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1737
_refine_ls_wR_factor_ref         0.1848
_reflns_Friedel_coverage         0.552
_reflns_Friedel_fraction_full    0.581
_reflns_Friedel_fraction_max     0.557
_reflns_number_gt                11636
_reflns_number_total             17444
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj04729k2.cif
_cod_data_source_block           jmp_tr_etyl_22
_cod_depositor_comments
;
The following automatic conversions were performed:
data name '__diffrn_detector_area_resol_mean' replaced with
'_diffrn_detector_area_resol_mean'.

Automatic conversion script
Id: cif_correct_tags 4968 2017-02-21 14:55:21Z antanas 

 Adding full bibliography for 7057074--7057075.cif.
;
_cod_database_code               7057075
_shelx_estimated_absorpt_t_min   0.871
_shelx_estimated_absorpt_t_max   0.891
_shelxl_version_number           2013-3
_shelx_res_checksum              49990