Chiral recognition between host and guest: a binaphthyl-18-crown-6 host with <small>D</small>-phenylglycinium methyl ester perchlorate guest. A difficult structure solved with <i>CRUNCH</i>
Cram, Donald J.; de Graaff, R. A. G.; Knobler, Carolyn B.; Lingenfelter, David S.; Maverick, Emily F.; Trueblood, Kenneth N.; Acta Crystallographica Section B 55 (1999) 432–440; doi:10.1107/S0108768198013524

data_2002986
_publ_section_title
;
 Chiral recognition between host and guest: a binaphthyl-18-crown-6
 host with <small>D</small>-phenylglycinium methyl ester perchlorate
 guest. A difficult structure solved with <i>CRUNCH</i>
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              432
_journal_page_last               440
_journal_paper_doi               10.1107/S0108768198013524
_journal_volume                  55
_journal_year                    1999
_chemical_formula_moiety         ' C42 H40 O6, C9 H12 N O2, Cl O4, H2 O'
_chemical_formula_sum            'C51 H52 Cl N O13'
_chemical_formula_weight         924.44
_chemical_melting_point          420(2)
_chemical_name_common            D20P
_chemical_name_systematic
;1:1 complex of
 (R)-2,3:4,5-bis[1,2-(3-phenylnaphtho)]-1,6,9,12,15,18-hexaoxacycloeicosa-2,4-
 diene with phenylglycinium methyl ester perchlorate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.048(7)
_cell_length_b                   34.383(6)
_cell_length_c                   11.992(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    175
_cell_measurement_theta_max      10.0
_cell_measurement_theta_min      7.95
_cell_volume                     9503(6)
_computing_cell_refinement       'UCLA CRYSTALLOGRAPHIC PACKAGE'
_computing_data_collection       'UCLA CRYSTALLOGRAPHIC PACKAGE'
_computing_data_reduction        'UCLA CRYSTALLOGRAPHIC PACKAGE'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1995)'
_computing_publication_material
'CRUNCH (preproduction version; de Graaff, 1998)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution
'CRUNCH (preproduction version; de Graaff, 1998)'
_diffrn_ambient_temperature      175(2)
_diffrn_measurement_device       'Rigaku AFC5R'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed  tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.14
_diffrn_reflns_av_sigmaI/netI    0.0648
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7823
_diffrn_reflns_theta_max         60.09
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        4
_diffrn_standards_interval_count 147
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.261
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_meas
; 1.261 Mg m^-3^ at 295 K.  The unit-cell volume at this temperature is
  9753; correcting  for the difference in volume at 175 K leads to a
  calculated density at 175 K of 1.294
;
_exptl_crystal_density_method    'flotation (carbon tetrachloride/benzene)'
_exptl_crystal_description       'cut needle'
_exptl_crystal_F_000             3904
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.032
_refine_diff_density_min         -0.590
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   -0.14(4)
_refine_ls_extinction_coef       0.00111(12)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.003
_refine_ls_goodness_of_fit_obs   1.010
_refine_ls_hydrogen_treatment
;
 H atoms riding; fixed C-H distances,<u^2^>~H~ = 1.2 times U~eq~ of
 attached C, except for CH~3~ and NH~3~^+^ groups, for which factor
 was 1.5; CH~3~ groups rotating about O-C bond; NH~3~^+^ groups rotating
 about C-N bond
;
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1208
_refine_ls_number_reflns         7784
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.001
_refine_ls_restrained_S_obs      1.007
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_obs          0.0793
_refine_ls_shift/esd_max         0.051,0.342,0.287
_refine_ls_shift/esd_mean        0.005,0.039,0.044
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1470P)^2^+18.9318P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2247
_refine_ls_wR_factor_obs         0.2112
_reflns_number_observed          6928
_reflns_number_total             7821
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            fr0005.cif
_cod_data_source_block           Text
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1470P)^2^+18.9318P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1470P)^2^+18.9318P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C51 H52 Cl1 N1 O13'
_cod_database_code               2002986
_cod_database_fobs_code          2002986