A macrocycle directed total synthesis of di-O-methylendiandrin A.
Barnes, Timothy H.; Johnson, Kara F.; Gorden, John D.; Merner, Bradley L.; Chemical communications (Cambridge, England) 56 (2020) 8747–8749; doi:10.1039/d0cc03302b

data_7126644
_publ_section_title
;
 A macrocycle directed total synthesis of di-O-methylendiandrin A.
;
_journal_issue                   62
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8747
_journal_page_last               8749
_journal_paper_doi               10.1039/d0cc03302b
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         ' C26H32O6'
_chemical_formula_sum            'C26 H32 O6'
_chemical_formula_weight         440.51
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2019-07-05 deposited with the CCDC.	2020-06-04 downloaded from the CCDC.
;
_cell_angle_alpha                98.2020(10)
_cell_angle_beta                 99.4460(10)
_cell_angle_gamma                90.5440(10)
_cell_formula_units_Z            4
_cell_length_a                   7.3978(2)
_cell_length_b                   17.6152(4)
_cell_length_c                   18.2995(5)
_cell_measurement_reflns_used    9843
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      74.4886
_cell_measurement_theta_min      3.7945
_cell_volume                     2326.96(10)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection
'Bruker Instrument Service, BIS, v6.2.6 (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 882)'
_computing_publication_material  'APEX3 v2018.1-0 (Bruker AXS Inc., 2017)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            86797
_diffrn_reflns_theta_full        74.54
_diffrn_reflns_theta_max         74.54
_diffrn_reflns_theta_min         2.47
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Incoatec I\mS DIAMOND'
_exptl_absorpt_coefficient_mu    0.719
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.093
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.228
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         9475
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0419P)^2^+0.9088P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0880
_reflns_number_gt                8605
_reflns_number_total             9475
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03302b2.cif
_cod_data_source_block           Merner061219
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

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

 Adding full bibliography for 7126644.cif.
;
_cod_database_code               7126644
_shelx_res_checksum              93382
_shelx_hkl_checksum              15164