Crystalline sponge X-ray analysis coupled with supercritical fluid chromatography: a novel analytical platform for the rapid separation, isolation, and characterization of analytes.
Taniguchi, Yoshimasa; Miwa, Mayuka; Kitada, Naoki; The Analyst 146 (2021) 5230–5235; doi:10.1039/d1an00948f

data_1564347
_publ_section_title
;
 Crystalline sponge X-ray analysis coupled with supercritical fluid
 chromatography: a novel analytical platform for the rapid separation,
 isolation, and characterization of analytes.
;
_journal_issue                   17
_journal_name_full               'The Analyst'
_journal_page_first              5230
_journal_page_last               5235
_journal_paper_doi               10.1039/d1an00948f
_journal_volume                  146
_journal_year                    2021
_chemical_absolute_configuration rmad
_chemical_formula_moiety
;
(C46 H38 Co2 N6 O6), (C14 H14 O2), 2(N O3), (C2 H3 N), 0.236(O)
;
_chemical_formula_sum            'C62 H55 Co2 N9 O14.23'
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_space_group_crystal_system      monoclinic
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;
2021-02-11 deposited with the CCDC.	2021-02-11 downloaded from the CCDC.
;
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_cell_measurement_temperature    100.01(10)
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_cell_volume                     2915.02(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
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_computing_molecular_graphics    'shelXle (Hubschle et al., 2011)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
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_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
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_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 1.000
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_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
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_diffrn_reflns_point_group_measured_fraction_full 1.000
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_exptl_absorpt_coefficient_mu    5.097
_exptl_absorpt_correction_T_max  0.839
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_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_description       block
_exptl_crystal_F_000             1316
_exptl_crystal_size_max          0.161
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.068
_refine_diff_density_max         2.090
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details
;
 Flack x determined using 4641 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.011(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_reflns         11510
_refine_ls_number_restraints     907
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0681
_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^)+(0.1079P)^2^+3.7014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1809
_refine_ls_wR_factor_ref         0.1821
_reflns_Friedel_coverage         0.927
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.946
_reflns_number_gt                11213
_reflns_number_total             11510
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1an00948f1.cif
_cod_data_source_block           6c@3R
_cod_depositor_comments
'Adding full bibliography for 1564341--1564354.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1564347
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.494
_shelx_estimated_absorpt_t_max   0.723
_shelx_res_checksum              20826
_shelx_hkl_checksum              60094