Selective Formation of Chromogen I from N-Acetyl-d-glucosamine upon Lanthanide Coordination.
Zheng, Xiu-Ying; Peng, Jun-Bo; Livera, M M Varuni S; Luo, Yun; Wang, Ya-Yun; Kong, Xiang-Jian; Long, La-Sheng; Zheng, Zhiping; Zheng, Lan-Sun; Inorganic chemistry 56 (2017) 110–113; doi:10.1021/acs.inorgchem.6b02589

data_4344942
_publ_section_title
;
 Selective Formation of Chromogen I from N-Acetyl-d-glucosamine upon
 Lanthanide Coordination.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              110
_journal_page_last               113
_journal_paper_doi               10.1021/acs.inorgchem.6b02589
_journal_volume                  56
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_sum            'C40 H138 Cl5 Gd9 N4 O94'
_chemical_formula_weight         3772.03
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      cubic
_space_group_IT_number           195
_space_group_name_Hall           'P 2 2 3'
_space_group_name_H-M_alt        'P 2 3'
_symmetry_space_group_name_Hall  'P 2 2 3'
_symmetry_space_group_name_H-M   'P 2 3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   43.0069(3)
_cell_length_b                   43.0069(3)
_cell_length_c                   43.0069(3)
_cell_measurement_reflns_used    25310
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.0627
_cell_measurement_theta_min      2.7561
_cell_volume                     79545.3(10)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1616
_diffrn_reflns_av_unetI/netI     0.2113
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            194042
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.990
_diffrn_reflns_theta_min         2.762
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.639
_exptl_absorpt_correction_T_max  0.2935
_exptl_absorpt_correction_T_min  0.2935
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro, Agilent Technologies'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.890
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             43656
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_platon_squeeze_details
;
;
_refine_diff_density_max         2.898
_refine_diff_density_min         -0.977
_refine_diff_density_rms         0.209
_refine_ls_abs_structure_details
;
 Flack x determined using 5691 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.064(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1838
_refine_ls_number_reflns         46425
_refine_ls_number_restraints     847
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.1621
_refine_ls_R_factor_gt           0.0953
_refine_ls_shift/su_max          0.057
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1021P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2250
_refine_ls_wR_factor_ref         0.2609
_reflns_Friedel_coverage         0.906
_reflns_Friedel_fraction_full    0.961
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                21751
_reflns_number_total             46425
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02589_si_002.cif
_cod_data_source_block           Gd9
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 4344941--4344942.cif.

2020-06-09
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C80 H276 Cl10 Gd18 N8 O188'
_cod_original_formula_weight         7544.07
_cod_original_formula_units_Z            12
_cod_original_cell_volume        79545.3(17)
_cod_database_code               4344942
_shelx_estimated_absorpt_t_min   0.294
_shelx_estimated_absorpt_t_max   0.337
_platon_gd9_details
;
SQUEEZE removed 10 disordered ClO4- anions and 50 disordered 
water molecules per formula unit. This valueis calculated 
based upon elemental analysis data.
;
_shelxl_version_number           2013-2
_shelx_res_checksum              14128
_shelx_hkl_checksum              94725