A new class of three dimensional D-π-A trigonal cryptand derivatives for second-order nonlinear optics
Mukhopadhyay, Pritam; Bharadwaj, Parimal K.; Savitha, G.; Krishnan, Anu; Das, Puspendu K.; Journal of Materials Chemistry 12 (2002) 2237–; doi:10.1039/b202770b

data_7204418
_publ_section_title
;
 A new class of three dimensional D-\p-A trigonal cryptand
 derivatives for second-order nonlinear optics
;
_journal_issue                   8
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              2237
_journal_paper_doi               10.1039/b202770b
_journal_volume                  12
_journal_year                    2002
_chemical_formula_moiety         'C53 H54 N12 O15'
_chemical_formula_sum            'C53 H54 N12 O15'
_chemical_formula_weight         1099.08
_chemical_melting_point          433.15
_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                89.51(6)
_cell_angle_beta                 79.11(2)
_cell_angle_gamma                75.62(4)
_cell_formula_units_Z            2
_cell_length_a                   11.798(2)
_cell_length_b                   12.137(7)
_cell_length_c                   19.707(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.6
_cell_measurement_theta_min      9.7
_cell_volume                     2682.1(19)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms and Wocadlo, 1995)'
_computing_molecular_graphics    ORTEP3
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    xtal
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Enraf Nonius Turbo CAD4'
_diffrn_measurement_method       theta-2theta
_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  0.1040
_diffrn_reflns_av_sigmaI/netI    0.3072
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7391
_diffrn_reflns_theta_full        22.48
_diffrn_reflns_theta_max         22.48
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        'less than 0.7%'
_diffrn_standards_interval_time  'every hour'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.102
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_meas      1.38
_exptl_crystal_density_method    floatation
_exptl_crystal_description       'rectangular parallelopiped'
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       0.0054(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.935
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     638
_refine_ls_number_reflns         6980
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.935
_refine_ls_R_factor_all          0.3104
_refine_ls_R_factor_gt           0.0840
_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^)+(0.1664P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2234
_refine_ls_wR_factor_ref         0.3421
_reflns_number_gt                1941
_reflns_number_total             6980
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b202770b.txt
_cod_data_source_block           L4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '160 celcius' was changed to '433.15'
- it was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        2682.0(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7204418