Determination of the critical chain length for macromolecular crystallization using structurally flexible polyketones
Ide, Yuki; Manabe, Yumehiro; Inaba, Yuya; Kinoshita, Yusuke; Pirillo, Jenny; Hijikata, Yuh; Yoneda, Tomoki; Shivakumar, Kilingaru I.; Tanaka, Saki; Asakawa, Hitoshi; Inokuma, Yasuhide; Chemical Science  (2022) –; doi:10.1039/D2SC03083G

data_1567278
_publ_section_title
;
 Determination of the critical chain length for macromolecular
 crystallization using structurally flexible polyketones
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC03083G
_journal_year                    2022
_chemical_formula_moiety         'C35 H52 O10'
_chemical_formula_sum            'C35 H52 O10'
_chemical_formula_weight         632.76
_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_creation_method           SHELXL-2019/2
_audit_update_record
;
2022-05-20 deposited with the CCDC.	2022-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4486(3)
_cell_length_b                   8.0259(2)
_cell_length_c                   41.6406(12)
_cell_measurement_reflns_used    11819
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      73.9630
_cell_measurement_theta_min      4.2120
_cell_volume                     3491.96(17)
_computing_cell_refinement       'CrysAlisPro 1.171.41.95a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.95a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.95a (Rigaku OD, 2021)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            33788
_diffrn_reflns_point_group_measured_fraction_full 0.944
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        67.494
_diffrn_reflns_theta_max         67.494
_diffrn_reflns_theta_min         2.122
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    0.713
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42126
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.95a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.830
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.943
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.123
_refine_ls_abs_structure_details
;
 Flack x determined using 1887 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.1(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         5956
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.1381
_refine_ls_R_factor_gt           0.1315
_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^)+(0.2931P)^2^+3.0700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4029
_refine_ls_wR_factor_ref         0.4120
_reflns_Friedel_coverage         0.865
_reflns_Friedel_fraction_full    0.889
_reflns_Friedel_fraction_max     0.889
_reflns_number_gt                5027
_reflns_number_total             5956
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc03083g2.cif
_cod_data_source_block           pentamer
_cod_database_code               1567278
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_min   0.589
_shelx_estimated_absorpt_t_max   0.958
_shelx_res_checksum              17574