A Self-assembled, Metalloorganic Supramolecular Frequency Doubler
Luke A. Burke; Grazia Gonella; Fenton Heirtzler; Hai-Lung Dai; Stephanie Jones; Jon Zubieta; Alex J. Roche; Chem.Commun. 48 (2012) 1000–; doi:10.1039/c2cc16199k

data_7107209
_publ_section_title
;
 A Self-assembled, Metalloorganic Supramolecular Frequency Doubler
;
_journal_name_full               Chem.Commun.
_journal_page_first              1000
_journal_paper_doi               10.1039/c2cc16199k
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C46 H26 Cu2 N14 O8, 2(F6 P), 3(C2 H3 N)'
_chemical_formula_sum            'C56 H41 Cu2 F12 N19 O8 P2'
_chemical_formula_weight         1525.10
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                72.940(4)
_cell_angle_beta                 82.840(4)
_cell_angle_gamma                78.612(4)
_cell_formula_units_Z            2
_cell_length_a                   9.4377(16)
_cell_length_b                   15.912(3)
_cell_length_c                   20.940(3)
_cell_measurement_reflns_used    14004
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.08
_cell_measurement_theta_min      1.02
_cell_volume                     2939.6(9)
_computing_cell_refinement       'Bruker SMART (Bruker, 2002)'
_computing_data_collection       'Bruker SMART (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2002)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2006)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2002)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_av_sigmaI/netI    0.1214
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29016
_diffrn_reflns_theta_full        28.08
_diffrn_reflns_theta_max         28.08
_diffrn_reflns_theta_min         1.02
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0.001
_exptl_absorpt_coefficient_mu    0.891
_exptl_absorpt_correction_T_max  0.9321
_exptl_absorpt_correction_T_min  0.8419
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS SHELXL-97 (Sheldrick, 1997)'
_exptl_crystal_density_diffrn    1.723
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1540
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;The unit cell contains 2 acetonitirle molecules which have been treated
as a diffuse contribution to the overall scattering without specific arom
positions by SQUEEZE/PLATON in addition to the 3 acetonitrile molecules
found in the electron density map.

Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_diff_density_max         0.832
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     841
_refine_ls_number_reflns         14004
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.1300
_refine_ls_R_factor_gt           0.0672
_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^)+(0.0815P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1543
_refine_ls_wR_factor_ref         0.1773
_reflns_number_gt                7628
_reflns_number_total             14004
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc16199k.txt
_cod_data_source_block           p-1[2]
_cod_original_cell_volume        2939.5(9)
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7107209