Expansion by Contraction: Diversifying the Photochemical Reactivity Scope of Diazo-oxochlorins toward Development of in Situ Alkylating Agents
Tillmann Köpke; Maren Pink; Jeffrey M. Zaleski; Journal of the American Chemical Society 130 (2008) 15864–15871; doi:10.1021/ja800094e

data_4108695
_publ_section_title
;
 Expansion by Contraction: Diversifying the Photochemical Reactivity Scope
 of Diazo-oxochlorins toward Development of in Situ Alkylating Agents
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15864
_journal_page_last               15871
_journal_paper_doi               10.1021/ja800094e
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C51 H36 Cu N6 O3 S, 1.5 C4 H10 O'
_chemical_formula_sum            'C57 H51 Cu N6 O4.5 S'
_chemical_formula_weight         987.64
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.302(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.121(4)
_cell_length_b                   10.4755(15)
_cell_length_c                   18.364(3)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    95(2)
_cell_measurement_theta_max      20.1
_cell_measurement_theta_min      2.5
_cell_volume                     4721.6(13)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2003), XTEL (loc. libr.)'
_computing_publication_material  'SHELXTL (Bruker, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      95(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details      '0.5 degree frames measured for 1 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'diamond 1 1 1'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.49595
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            81662
_diffrn_reflns_theta_full        20.14
_diffrn_reflns_theta_max         20.14
_diffrn_reflns_theta_min         1.16
_exptl_absorpt_coefficient_mu    0.304
_exptl_absorpt_correction_T_max  0.9970
_exptl_absorpt_correction_T_min  0.9559
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing; 1995'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_description       needle
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.210
_refine_diff_density_min         -1.410
_refine_diff_density_rms         0.359
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     654
_refine_ls_number_reflns         12991
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.195
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1004P)^2^+0.8989P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1381
_refine_ls_wR_factor_ref         0.1569
_reflns_number_gt                11464
_reflns_number_total             12991
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja800094e_si_002.cif
_cod_data_source_block           0517
_cod_original_cell_volume        4721.7(13)
_cod_original_formula_sum        'C57 H51 Cu N6 O4.50 S'
_cod_database_code               4108695