Preparation of the tricyclic ketopyrrole core of roseophilin by radical macrocyclisation and Paal–Knorr condensation
Robertson, Jeremy; Hatley, Richard J. D.; Watkin, David J.; Journal of the Chemical Society, Perkin Transactions 1  (2000) 3389–; doi:10.1039/b005351l

data_7213410
_publ_section_title
;
 Preparation of the tricyclic ketopyrrole core of roseophilin by radical
 macrocyclisation and Paal--Knorr condensation
;
_journal_issue                   20
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              3389
_journal_paper_doi               10.1039/b005351l
_journal_year                    2000
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C18 H30 O2 '
_chemical_formula_sum            'C18 H30 O2'
_chemical_formula_weight         278.44
_chemical_melting_point          ?
_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
_audit_creation_date             99-05-11
_audit_creation_method           CRYSTALS_ver_12-03-99
_cell_angle_alpha                94.724(11)
_cell_angle_beta                 99.273(16)
_cell_angle_gamma                97.332(13)
_cell_formula_units_Z            2
_cell_length_a                   6.3717(14)
_cell_length_b                   10.2304(11)
_cell_length_c                   12.680(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    177
_cell_measurement_theta_max      43
_cell_measurement_theta_min      21
_cell_volume                     804.6(2)
_computing_cell_refinement       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_reduction
;
RC93 (Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. 1994)
;
_computing_molecular_graphics
;
 CAMERON (Watkin, Prout & Pearce,  1996)
;
_computing_publication_material
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_computing_structure_refinement
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      177
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  '  Enraf-nonius CAD4 '
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.04
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7656
_diffrn_reflns_theta_max         74.33
_diffrn_reflns_theta_min         0.00
_diffrn_standards_decay_%        9.42
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.56
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '\y scan,(North et al, 1968)'
_exptl_crystal_colour            ' colourless '
_exptl_crystal_density_diffrn    1.15
_exptl_crystal_density_meas      ?
_exptl_crystal_description       ' lozenge '
_exptl_crystal_F_000             308.77
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.35
_refine_diff_density_min         -0.22
_refine_ls_extinction_coef       272.6(83)
_refine_ls_extinction_method     'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_ref   0.8606
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2906
_refine_ls_R_factor_gt           0.0517
_refine_ls_shift/su_max          0.000312
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 2 parameters, Carruthers & Watkin , 1979,
 4.34     4.65
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0550
_reflns_limit_h_max              7
_reflns_limit_h_min              -7
_reflns_limit_k_max              12
_reflns_limit_k_min              -12
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                2906
_reflns_number_total             3047
_reflns_threshold_expression     >3.00\s(I)
_cod_data_source_file            b005351lsup1.cif
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_symmetry_cell_setting' value
'Triclinic ' changed to 'triclinic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        804.6
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        ' C18 H30 O2 '
_cod_database_code               7213410