Synthesis of C<sub>70</sub>-fragment buckybowls bearing alkoxy substituents.
Yakiyama, Yumi; Hishikawa, Shota; Sakurai, Hidehiro; Beilstein journal of organic chemistry 16 (2020) 681–690; doi:10.3762/bjoc.16.66

data_4038256
_publ_section_title
;
 Synthesis of C<sub>70</sub>-fragment buckybowls bearing alkoxy
 substituents.
;
_journal_name_full               'Beilstein journal of organic chemistry'
_journal_page_first              681
_journal_page_last               690
_journal_paper_doi               10.3762/bjoc.16.66
_journal_volume                  16
_journal_year                    2020
_chemical_formula_moiety         'C29 H14 O2'
_chemical_formula_sum            'C29 H14 O2'
_chemical_formula_weight         394.40
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-01-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.62(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.274(4)
_cell_length_b                   7.4408(15)
_cell_length_c                   27.913(6)
_cell_measurement_reflns_used    3950
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.37
_cell_measurement_theta_min      3.03
_cell_volume                     3526.3(14)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        PROCESS-AUTO
_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    'XS (Sheldrick, 2008)'?'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Rigaku R-AXIS VII area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1884
_diffrn_reflns_av_unetI/netI     0.3510
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            19291
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.026
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  0.9999
_exptl_absorpt_correction_T_min  0.5437
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_description       block
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.214
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         7995
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.3593
_refine_ls_R_factor_gt           0.1217
_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^)+(0.0558P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1498
_refine_ls_wR_factor_ref         0.2096
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2351
_reflns_number_total             7995
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Dioxole-5c-re.cif
_cod_data_source_block           Dioxole5c
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_cell_measurement_temperature' value '150(2' was changed
to '150(2)' -- precision was estimated.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 4038256--4038257.cif.
;
_cod_original_cell_volume        3526.2(13)
_cod_database_code               4038256
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 C23, C24, C25, C26, C27, C28
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 C23, C24
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C13(H13A,H13B), C29(H29A,H29B), C37(H37A,H37B), C42(H42A,H42B),
 C58(H58A,H58B)
5.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C15(H15), C16(H16), C18(H18), C22(H22), C25(H25),
 C26(H26), C39(H39), C40(H40), C44(H44), C45(H45), C47(H47), C51(H51), C54(H54),
  C55(H55)
;
_olex2_submission_special_instructions 'No special instructions were received'