Electrochemical and Structural Investigation of the Interactions between Naphthalene Diimides and Metal Cations
Reiner, Benjamin R.; Foxman, Bruce M.; Wade, Casey R.; Dalton Trans.  (2017) –; doi:10.1039/C7DT02067H

data_7043491
_publ_section_title
;
 Electrochemical and Structural Investigation of the Interactions between
 Naphthalene Diimides and Metal Cations
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02067H
_journal_year                    2017
_chemical_formula_moiety         'C100 H124.00 Mg2 N4 O14'
_chemical_formula_sum            'C100 H124 Mg2 N4 O14'
_chemical_formula_weight         1654.71
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2017-02-06
_audit_creation_method           CRYSTALS_ver_14.61_build_00000
_audit_update_record
;
2017-03-20 deposited with the CCDC.
2017-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.5029(15)
_cell_length_b                   19.1115(14)
_cell_length_c                   27.069(2)
_cell_measurement_reflns_used    5037
_cell_measurement_temperature    120
_cell_measurement_theta_max      20
_cell_measurement_theta_min      2
_cell_volume                     11124.1(14)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_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    'USER DEFINED STRUCTURE SOLUTION'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_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  0.072
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8257
_diffrn_reflns_theta_full        23.534
_diffrn_reflns_theta_max         23.534
_diffrn_reflns_theta_min         1.505
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    0.988
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3552.002
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.220
_platon_squeeze_details
;
TITL brr_93_0ma in Pbca
CELL   21.5030   19.1110   27.0690     90.00     90.00     90.00
SPGR Pbca
Q101 0.953 0.182 0.400 !       2.34 eA-3
C102 0.992 0.749 0.059 !       2.28 eA-3
C103 0.756 0.033 0.368 !       2.11 eA-3
Q104 0.267 0.724 0.163 !       2.01 eA-3
C105 0.538 0.703 0.437 !       1.83 eA-3
C106 0.258 1.002 0.060 !       1.82 eA-3
C107 0.492 0.197 0.146 !       1.81 eA-3
C108 0.265 0.517 0.114 !       1.79 eA-3
C109 0.479 0.729 0.402 !       1.75 eA-3
C110 0.788 0.010 0.365 !       1.71 eA-3
C111 0.982 0.184 0.472 !       1.49 eA-3
C112 0.767 0.583 0.381 !       1.46 eA-3
C113 0.984 0.530 0.978 !       1.45 eA-3
Q114 0.758 0.299 0.312 !       1.42 eA-3
Q115 0.405 0.176 0.090 !       1.39 eA-3
C116 0.221 0.062 0.058 !       1.38 eA-3
Q117 0.773 0.810 0.400 !       1.29 eA-3
C118 0.674 0.533 0.397 !       1.29 eA-3
C119 0.483 0.986 0.978 !       1.26 eA-3
Q120 0.246 0.662 0.137 !       1.21 eA-3
C121 0.182 0.465 0.119 !       1.20 eA-3
Q122 0.766 0.846 0.301 !       1.14 eA-3
Q123 0.757 0.828 0.376 !       1.13 eA-3
Q124 0.766 0.298 0.346 !       1.08 eA-3
C125 0.203 0.422 0.097 !       1.07 eA-3
Q126 0.391 0.268 0.623 !       1.05 eA-3
C127 0.312 0.974 0.074 !       1.04 eA-3
C128 0.923 0.140 0.451 !       0.97 eA-3
C129 0.947 0.956 0.462 !       0.96 eA-3
C130 0.030 0.517 0.039 !       0.86 eA-3
C131 0.014 0.417 0.049 !       0.80 eA-3
C132 0.429 0.012 0.017 !       0.79 eA-3
Q133 0.775 0.329 0.904 !       0.73 eA-3
Q134 0.634 0.864 0.266 !       0.72 eA-3
C135 0.696 0.518 0.906 !       0.68 eA-3
Q136 0.689 0.623 0.433 !       0.67 eA-3
C137 0.729 0.388 0.379 !       0.67 eA-3
C138 0.289 0.777 0.203 !       0.63 eA-3
Q139 0.980 0.241 0.876 !       0.63 eA-3
Q140 0.111 0.610 0.103 !       0.63 eA-3
Q141 0.705 0.594 0.412 !       0.63 eA-3
C142 0.639 0.443 0.417 !       0.62 eA-3
Q143 0.827 0.091 0.388 !       0.58 eA-3
Q144 0.719 0.895 0.877 !       0.58 eA-3
Q145 0.681 0.185 0.902 !       0.57 eA-3
C146 0.248 0.072 0.156 !       0.57 eA-3
Q147 0.873 0.345 0.751 !       0.56 eA-3
Q148 0.664 0.769 0.359 !       0.55 eA-3
Q149 0.632 0.894 0.945 !       0.55 eA-3
Q150 0.569 0.767 0.951 !       0.55 eA-3
C151 0.312 0.635 0.658 !       0.54 eA-3
Q152 0.704 0.860 0.850 !       0.53 eA-3
C153 0.487 0.402 0.488 !       0.52 eA-3
C154 0.209 0.405 0.169 !       0.52 eA-3
C155 0.837 0.876 0.421 !       0.52 eA-3
C156 0.626 0.106 0.898 !       0.50 eA-3
;
_refine_diff_density_max         1.07
_refine_diff_density_min         -0.70
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9786
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         8241
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.1471
_refine_ls_R_factor_gt           0.0892
_refine_ls_shift/su_max          0.0081031
_refine_ls_shift/su_mean         0.0004751
_refine_ls_structure_factor_coef Fsqd
_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: 
 15.3 23.6 11.0 2.60 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2899
_refine_ls_wR_factor_gt          0.2307
_refine_ls_wR_factor_ref         0.2899
_reflns_limit_h_max              24
_reflns_limit_h_min              0
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                4323
_reflns_number_total             8257
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.1471
_oxford_refine_ls_scale          0.050792(18)
_oxford_reflns_number_all        8241
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'brr_93_0ma in Pbca'
_cod_data_source_file            c7dt02067h2.cif
_cod_data_source_block           brr_93
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_sg_symbol_H-M      'P b c a '
_cod_original_formula_sum        'C100 H124.00 Mg2 N4 O14'
_cod_database_code               7043491
_platon_squeeze_void_probe_radius 1.20