Hierarchical multicomponent assembly utilizing sequential metal‒ligand and hydrogen-bonding interactions
Constable, Edwin C.; Zhang, Guoqi; Housecroft, Catherine E.; Neuburger, Markus; Schaffner, Silvia; CrystEngComm 11 (2009) 657–662; doi:10.1039/b817706f

data_7200543
_publ_section_title
;
 Hierarchical multicomponent assembly utilizing sequential metal--ligand
 and hydrogen-bonding interactions
;
_journal_coden_ASTM              CRECF4
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              657
_journal_page_last               662
_journal_paper_doi               10.1039/b817706f
_journal_volume                  11
_journal_year                    2009
_chemical_absolute_configuration ad
_chemical_formula_moiety         '2(C24 H28 Cu N2 O4), C12 H8 O4, 2(H2 O)'
_chemical_formula_sum            'C60 H68 Cu2 N4 O14'
_chemical_formula_weight         1196.31
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             08-09-01
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 104.532(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.2898(8)
_cell_length_b                   7.7309(4)
_cell_length_c                   22.0964(11)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    123
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     2693.7(2)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      123
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            28759
_diffrn_reflns_theta_full        25.268
_diffrn_reflns_theta_max         28.075
_diffrn_reflns_theta_min         2.015
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.863
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_description       needle
_exptl_crystal_F_000             1252
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.34
_refine_diff_density_min         -0.52
_refine_ls_abs_structure_details 'Flack (1983), 5561 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.010(12)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1162
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     740
_refine_ls_number_reflns         7434
_refine_ls_number_restraints     35
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.000268
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.625 -0.247E-01 0.339
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0558
_refine_ls_wR_factor_gt          0.0310
_refine_ls_wR_factor_ref         0.0310
_reflns_limit_h_max              20
_reflns_limit_h_min              -21
_reflns_limit_k_max              10
_reflns_limit_k_min              -9
_reflns_limit_l_max              29
_reflns_limit_l_min              0
_reflns_number_gt                7434
_reflns_number_total             12470
_reflns_threshold_expression     I>3.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.3088(2)
_oxford_structure_analysis_title 'gq19_2_123k_0m in P2(1)'
_cod_data_source_file            B817706F.txt
_cod_data_source_block           gq19_2_123k
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

 Replaced the incorrect bibliographical reference to the original
 publication with a proper one.

 Antanas Vaitkus,
 2019-09-18
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7200543