Circular dichroism spectroscopy of catalyst preequilibrium in asymmetric autocatalysis of pyrimidyl alkanol.
Matsumoto, Arimasa; Tanaka, Ayame; Kaimori, Yoshiyasu; Hara, Natsuki; Mikata, Yuji; Soai, Kenso; Chemical communications (Cambridge, England) 57 (2021) 11209–11212; doi:10.1039/d1cc04206h

data_7129068
_publ_section_title
;
 Circular dichroism spectroscopy of catalyst preequilibrium in asymmetric
 autocatalysis of pyrimidyl alkanol.
;
_journal_issue                   85
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11209
_journal_page_last               11212
_journal_paper_doi               10.1039/d1cc04206h
_journal_volume                  57
_journal_year                    2021
_chemical_absolute_configuration rmad
_chemical_formula_sum            'C44 H62 N6 O2 Zn2'
_chemical_formula_weight         776.25
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-07-26 deposited with the CCDC.	2021-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0737(12)
_cell_length_b                   19.301(2)
_cell_length_c                   23.277(3)
_cell_measurement_reflns_used    5222
_cell_measurement_temperature    100
_cell_measurement_theta_max      23.92
_cell_measurement_theta_min      2.20
_cell_volume                     4525.8(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics
'Shelxle (J. Appl. Cryst., 44, (2011) 1281-1284.)'
_computing_publication_material
'Shelxle (J. Appl. Cryst., 44, (2011) 1281-1284.)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_source         'fine-focus rotational anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0650
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20738
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.485
_diffrn_reflns_theta_max         24.485
_diffrn_reflns_theta_min         1.371
_exptl_absorpt_coefficient_mu    1.097
_exptl_absorpt_correction_T_max  0.8889
_exptl_absorpt_correction_T_min  0.8528
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS; Sheldrick 1996
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prysm
_exptl_crystal_F_000             1532
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.687
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 2441 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.013(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         7503
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0441P)^2^+0.4886P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0948
_reflns_Friedel_coverage         0.778
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                6473
_reflns_number_total             7503
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04206h2.cif
_cod_data_source_block           ZNpyridine480b
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

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

 Adding full bibliography for 7129068--7129069.cif.
;
_cod_original_cell_volume        4525.8(10)
_cod_database_code               7129068
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.853
_shelx_estimated_absorpt_t_max   0.889
_shelx_res_checksum              4779