Reactions of triene-conjugated diazo-compounds: reaction paths from o-(1,3-dienyl)aryldiazomethanes to 3,8-methano-1,2-diazocines and to pyrrolo[2,1-a]phthalazines via intramolecular (3 + 2) and 1,1-cycloaddition reactions
Sharp, John T.; Wilson, Paul; Parsons, Simon; Gould, Robert O.; Journal of the Chemical Society, Perkin Transactions 1  (2000) 1139–; doi:10.1039/a909516k

data_7213223
_publ_section_title
;
 Reactions of triene-conjugated diazo-compounds: reaction paths from
 o-(1,3-dienyl)aryldiazomethanes to 3,8-methano-1,2-diazocines and to
 pyrrolo[2,1-a]phthalazines via intramolecular (3&#x2005;+&#x2005;2) and
 1,1-cycloaddition reactions
;
_journal_issue                   7
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              1139
_journal_paper_doi               10.1039/a909516k
_journal_year                    2000
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C24 H20 N2 '
_chemical_formula_sum            'C24 H20 N2'
_chemical_formula_weight         336.44
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             97-08-19
_audit_creation_method           CRYSTALS
_cell_angle_alpha                90
_cell_angle_beta                 112.113(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4.00
_cell_length_a                   17.081(2)
_cell_length_b                   7.0507(8)
_cell_length_c                   16.116(2)
_cell_measurement_reflns_used    46
_cell_measurement_temperature    220
_cell_measurement_theta_max      22
_cell_measurement_theta_min      20
_cell_volume                     1798.1(4)
_computing_cell_refinement       DIF4
_computing_data_collection       DIF4
_computing_data_reduction        REDU4
_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      220
_diffrn_measurement_device
;
Stoe Stadi-4 diffractometer equipped
with an Oxford Cryosystems l.t. device.
;
_diffrn_measurement_method       'Omega-theta with learnt-profile (Clegg)'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.02
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4128
_diffrn_reflns_theta_max         70.08
_diffrn_reflns_theta_min         2.79
_diffrn_standards_decay_%        5.00
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.53
_exptl_crystal_colour            ' yellow '
_exptl_crystal_density_diffrn    1.24
_exptl_crystal_description       ' block '
_exptl_crystal_F_000             713.74
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.20
_refine_diff_density_min         -0.18
_refine_ls_extinction_coef       31.5(33)
_refine_ls_extinction_method     'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_obs   1.1246
_refine_ls_hydrogen_treatment
;
 H atoms placed geometrically after each cycle
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         2633
_refine_ls_R_factor_obs          0.0451
_refine_ls_shift/esd_max         0.001145
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme
;
 Chebychev polynomial (Carruthers & Watkin, 1979)
;
_refine_ls_wR_factor_obs         0.0475
_reflns_limit_h_max              19
_reflns_limit_h_min              -20
_reflns_limit_k_max              8
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_observed          2633
_reflns_number_total             3184
_reflns_observed_criterion       >2.00\s(I)
_cod_data_source_file            a909516ksup1.cif
_cod_data_source_block           pw0375
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic ' changed to 'monoclinic'
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:

'_atom_sites_solution_primary' value 'Direct_Methods' was changed to
'direct'.

'_atom_sites_solution_hydrogens' value 'Geometric' was changed to
'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        1798.11
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        ' C24 H20 N2 '
_cod_database_code               7213223