Two-step crystal engineering of porous nets from [Cr/3(mu/3-O)(RCO/2)6] and [Cu/3(mu/3-Cl)(RNH2)/6Cl/6] molecular building blocks
Sameh K. Elsaidi; Mona H. Mohamed; Lukasz Wojtas; Amy J. Cairns; Mohamed Eddaoudi; Michael J. Zaworotko; Chem.Commun. 49 (2013) 8154–; doi:10.1039/c3cc44133d

data_7109718
_publ_section_title
;
 Two-step crystal engineering of porous nets from [Cr/3(mu/3-O)(RCO/2)6]
 and [Cu/3(mu/3-Cl)(RNH2)/6Cl/6] molecular building blocks
;
_journal_name_full               Chem.Commun.
_journal_page_first              8154
_journal_paper_doi               10.1039/c3cc44133d
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C126 H161 Cl14 Cr9 Cu6 N18 O65.5'
_chemical_formula_weight         4321.27
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           193
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c 2'
_symmetry_space_group_name_H-M   'P 63/m c 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                120.00
_cell_formula_units_Z            2
_cell_length_a                   29.72(2)
_cell_length_b                   29.72(2)
_cell_length_c                   26.388(18)
_cell_measurement_temperature    100(2)
_cell_volume                     20185(2)
_computing_cell_refinement       'APEX2 (Bruker, 2010); SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2009);XPREP(Sheldrick,2008)'
_computing_publication_material  'APEX2 (Bruker, 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'BRUKER SMART APEXII CCD'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.40663
_diffrn_reflns_av_R_equivalents  0.1506
_diffrn_reflns_av_sigmaI/netI    0.1086
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7178
_diffrn_reflns_theta_full        8.06
_diffrn_reflns_theta_max         8.06
_diffrn_reflns_theta_min         0.91
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_T_max  0.9974
_exptl_absorpt_correction_T_min  0.9873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2003)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    0.711
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4390
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
Mixture of MeOH and CH2Cl2 solvents have been used. 
Water can be present as well.Possible formula would therefore be 
[(Cr3O)3(H2O)3 (C7H6NO2)18(Cu3ClCl6)2].23.5H2O.(xCH2Cl2,yMeOH,zH2O)
with total number of electrons from x,y,z solcents not exceeding 
1332 per formula unit. 
;
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         1228
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.1336
_refine_ls_R_factor_gt           0.0931
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1340P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2290
_refine_ls_wR_factor_ref         0.2452
_reflns_number_gt                731
_reflns_number_total             1228
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc44133d.txt
_cod_data_source_block           tp-PMBB-6-stp-1_0m
_cod_original_cell_volume        20192(24)
_cod_original_sg_symbol_H-M      P63/mcm
_cod_original_formula_sum        'C126 H161 Cl14 Cr9 Cu6 N18 O65.50'
_cod_database_code               7109718