A fluorite isoreticular series of porous framework complexes with tetrahedral ligands: new opportunities for azolate PCPs
Boldog, Ishtvan; Domasevitch, Konstantin; Maclaren, Jana K.; Heering, Christian; Makhloufi, Gamall; Janiak, Christoph; CrystEngComm 16 (2014) 148–; doi:10.1039/c3ce42162g

data_7213547
_publ_section_title
;
 A fluorite isoreticular series of porous framework complexes with
 tetrahedral ligands: new opportunities for azolate PCPs
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              148
_journal_paper_doi               10.1039/c3ce42162g
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety
;
(Cu 2+)6, (Cl -)4, (C38 H28 N16 4-)2
;
_chemical_formula_sum            'C76 H56 Cl4 Cu6 N32'
_chemical_formula_weight         1940.57
_chemical_name_systematic
; 
 catena-(bis(\m~8~-(5,5',5'',5'''-((adamantane-1,3,5,7-tetrayl)-
-tetra-(phen-4-yl))-tetrakistetrazolato))-
 -(\m~4~-chloro)-trichloro-tetra-(N,N-dimethylacetamide)-
hexa-copper(ii), 
dimethylacetamide, methanol and water solvate
;
_space_group_IT_number           139
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4 2'
_symmetry_space_group_name_H-M   'I 4/m m m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.9532(3)
_cell_length_b                   18.9532(3)
_cell_length_c                   31.3238(12)
_cell_measurement_temperature    100(2)
_cell_volume                     11252.3(5)
_computing_cell_refinement       'Bruker APEXII'
_computing_data_collection       'Bruker APEXII'
_computing_data_reduction        'Bruker APEXII'
_computing_molecular_graphics    'DIAMOND (Crystal Impact, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart Apex CCD system'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0970
_diffrn_reflns_av_sigmaI/netI    0.0351
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            77075
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         1.26
_exptl_absorpt_coefficient_mu    0.628
_exptl_absorpt_correction_T_max  0.9399
_exptl_absorpt_correction_T_min  0.9341
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    0.573
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1956
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         3259
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1116P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1568
_refine_ls_wR_factor_ref         0.1673
_reflns_number_gt                2669
_reflns_number_total             3259
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce42162g.txt
_cod_data_source_block           Cu_AdPhThH4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/automatic-downloads/current/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 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      I4/mmm
_cod_database_code               7213547
_platon_calc_solv_details
;

 Total Potential Solvent Area Vol   7252.0 Ang^3
                  per Unit Cell Vol  11252.3 Ang^3 [64.4%]
 
Note: Expected volumes for solvent molecules are:
      A hydrogen bonded H2O-molecule      40 Ang^3
      Small molecules (e.g. Toluene) 100-300 Ang^3
 
      Values below for gridpoints and volumes in []
      refer to areas where atom centers may reside.
 
Area #GridPoint VolPerc.  Vol(A^3)  X(av) Y(av) Z(av) Eigenvector(frac) Sig(Ang)
 1 926587[571746] 64  7252[4474.8] -0.020 0.407-0.007 1  0.013 0.023 1.000  9.11
                                                      2  0.927 1.000-0.013  5.62
                                                      3 -1.000 0.927-0.003  5.37

Potential (!) solvent accessible voids for the structure with removed mu-4-Cl and disordered Cu2, Cl2 atoms, i.e. for the [Cu4L2] framework : 

Total Potential Solvent Area Vol   8665.0 Ang^3
                  per Unit Cell Vol  11252.3 Ang^3 [77.0%]
 
Note: Expected volumes for solvent molecules are:
      A hydrogen bonded H2O-molecule      40 Ang^3
      Small molecules (e.g. Toluene) 100-300 Ang^3
 
      Values below for gridpoints and volumes in []
      refer to areas where atom centers may reside.
 
:: Use the CALC SQUEEZE instruction to calculate and optionally correct for
:: Density identified in solvent accessible areas (Reflection data required)
 
Area #GridPoint VolPerc.  Vol(A^3)  X(av) Y(av) Z(av) Eigenvector(frac) Sig(Ang)
 11107116[775588] 77  8665[6070.2] -0.009-0.007-0.006 1  0.009 0.003 1.000  9.12
                                                      2  1.000 0.979-0.004  5.46
                                                      3 -0.979 1.000 0.002  5.41

 
;