Copper-catalyzed synthesis of spiro-indolofurobenzopyrans: tandem reactions of diazoamides and O-propargyl salicylaldehydes.
Muthusamy, Sengodagounder; Prabu, Ammasi; Suresh, Eringathodi; Organic & biomolecular chemistry 17 (2019) 8088–8093; doi:10.1039/c9ob01275c

data_7157040
_publ_section_title
;
 Copper-catalyzed synthesis of spiro-indolofurobenzopyrans: tandem
 reactions of diazoamides and O-propargyl salicylaldehydes.
;
_journal_issue                   35
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              8088
_journal_page_last               8093
_journal_paper_doi               10.1039/c9ob01275c
_journal_volume                  17
_journal_year                    2019
_chemical_formula_sum            'C48 H38 N2 O6'
_chemical_formula_weight         738.80
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
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_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
_audit_update_record
;
2017-10-15 deposited with the CCDC.    2019-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                91.650(2)
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_cell_angle_gamma                113.925(2)
_cell_formula_units_Z            2
_cell_length_a                   9.0014(13)
_cell_length_b                   9.5478(13)
_cell_length_c                   23.864(3)
_cell_measurement_reflns_used    7345
_cell_measurement_temperature    150(2)
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_cell_measurement_theta_min      2.34
_cell_volume                     1862.4(4)
_computing_cell_refinement       'BRUKER SMART'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        'BRUKER SAINT'
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'BRUKER SMART APEX CCD DIFFARCTOMETER'
_diffrn_measurement_method       'OMEGA-PHI SCAN'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
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_diffrn_reflns_limit_k_min       -11
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_diffrn_reflns_limit_l_min       -28
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_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  0.9828
_exptl_absorpt_correction_T_min  0.9644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCKS
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_refine_ls_number_reflns         6462
_refine_ls_number_restraints     0
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_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0399P)^2^+1.5515P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1249
_refine_ls_wR_factor_ref         0.1282
_reflns_number_gt                5683
_reflns_number_total             6462
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9ob01275c3.cif
_cod_data_source_block           samp43m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'TRICLINIC' changed to 'triclinic'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_refine_ls_hydrogen_treatment' value 'CONSTR' changed to 'constr'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7157040.cif.
;
_cod_original_cell_volume        1862.4(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7157040