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_1567279
_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         'C42 H62 O12'
_chemical_formula_sum            'C42 H62 O12'
_chemical_formula_weight         758.91
_space_group_crystal_system      orthorhombic
_space_group_IT_number           45
_space_group_name_Hall           'I 2 -2c'
_space_group_name_H-M_alt        'I b a 2'
_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                   48.930(9)
_cell_length_b                   8.2077(17)
_cell_length_c                   10.3345(18)
_cell_measurement_reflns_used    1032
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      50.7310
_cell_measurement_theta_min      5.4610
_cell_volume                     4150.4(14)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3983
_diffrn_reflns_point_group_measured_fraction_full 0.832
_diffrn_reflns_point_group_measured_fraction_max 0.831
_diffrn_reflns_theta_full        51.377
_diffrn_reflns_theta_max         51.377
_diffrn_reflns_theta_min         3.613
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.719
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.963
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.164
_refine_ls_abs_structure_details
;
 Flack x determined using 307 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.3(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.619
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         1893
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.608
_refine_ls_R_factor_all          0.2158
_refine_ls_R_factor_gt           0.1571
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3731
_refine_ls_wR_factor_ref         0.4353
_reflns_Friedel_coverage         0.588
_reflns_Friedel_fraction_full    0.668
_reflns_Friedel_fraction_max     0.668
_reflns_number_gt                1050
_reflns_number_total             1893
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc03083g2.cif
_cod_data_source_block           hexamer
_cod_database_code               1567279
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_min   0.772
_shelx_estimated_absorpt_t_max   0.993
_shelx_res_checksum              25381