Coordinating nature of M<sub>6</sub>L<sub>12</sub> double-stranded macrocycles: co-ligand competition of perchlorate, water, and acetonitrile depending on metal(II) ions.
An, Seonghyeon; Han, Jihun; Kim, Dongwon; Lee, Haeri; Jung, Ok-Sang; Dalton transactions (Cambridge, England : 2003) 53 (2024) 9692–9699; doi:10.1039/d4dt00902a

data_7716033
_publ_section_title
;
 Coordinating nature of M<sub>6</sub>L<sub>12</sub> double-stranded
 macrocycles: co-ligand competition of perchlorate, water, and
 acetonitrile depending on metal(II) ions.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9692
_journal_page_last               9699
_journal_paper_doi               10.1039/d4dt00902a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'C254 H332 Cl4 Co6 N31 O17 Si12, 8(Cl O4), 3(C7 H8)'
_chemical_formula_sum            'C273 H358 Cl12 Co6 N30 O50 Si12'
_chemical_formula_weight         5975.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-04-26 deposited with the CCDC.	2024-05-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.31(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.225(5)
_cell_length_b                   30.532(6)
_cell_length_c                   43.614(9)
_cell_measurement_reflns_used    547726
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      33.749
_cell_measurement_theta_min      0.458
_cell_volume                     34555(12)
_computing_cell_refinement       'Bruker APEX4 software'
_computing_data_collection       'Bruker APEX4 software'
_computing_data_reduction        'Bruker APEX4 software'
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Photon II detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.800
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0550
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            236697
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        28.685
_diffrn_reflns_theta_max         29.000
_diffrn_reflns_theta_min         1.742
_diffrn_source                   'Ius Microfocus'
_exptl_absorpt_coefficient_mu    0.658
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_description       block
_exptl_crystal_F_000             12560
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.830
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details
; 
 Flack x determined using 28385 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.5220(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     6394
_refine_ls_number_reflns         126449
_refine_ls_number_restraints     12431
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1167
_refine_ls_R_factor_gt           0.0913
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.001
_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          0.2628
_refine_ls_wR_factor_ref         0.2955
_reflns_Friedel_coverage         0.958
_reflns_Friedel_fraction_full    0.981
_reflns_Friedel_fraction_max     0.980
_reflns_number_gt                78968
_reflns_number_total             126449
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00902a2.cif
_cod_data_source_block           CoClO42_mDCPPS
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'MULTI-SCAN' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7716032--7716036.cif.

2024-09-24
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C546 H716 Cl24 Co12 N60 O100 Si24'
_cod_original_formula_weight         11951.87
_cod_original_formula_moiety
'C254 H332 Cl4 Co6 N31 O17 Si12, C250 H327 Cl4 Co6 N29 O19 Si12, 16(Cl O4), 6(C7 H8)'
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7716033
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.853
_shelx_estimated_absorpt_t_max   0.880
_shelx_res_checksum              31902
_shelx_fab_checksum              45178