Biladienones from the Photooxidation of ameso-gem-Disubstituted Phlorin: Crystal and Molecular Structures of the 3N + O Coordinated Nickel(II) and Copper(II) Complexes
Christophe Jeandon; Bénédicte Krattinger; Romain Ruppert; Henry J. Callot; Inorganic Chemistry 40 (2001) 3149–3153; doi:10.1021/ic001205b

data_4319852
_publ_section_title
;
 Biladienones from the Photooxidation of ameso-gem-Disubstituted Phlorin:
 Crystal and Molecular Structures of the 3N + O Coordinated Nickel(II) and
 Copper(II) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3149
_journal_page_last               3153
_journal_paper_doi               10.1021/ic001205b
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         'C48 H38 N4 Ni O2'
_chemical_formula_sum            'C48 H38 N4 Ni O2'
_chemical_formula_weight         761.57
_chemical_name_systematic        ' ?'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 101.546(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   41.726(3)
_cell_length_b                   9.1582(3)
_cell_length_c                   20.275(1)
_cell_measurement_temperature    294
_cell_volume                     7591.0(7)
_computing_publication_material  CIFGEN_IN_OpenMoleN_(_1997)
_computing_structure_refinement  LSFM_OpenMoleN_(_1997)
_computing_structure_solution    Direct_methods_(SIR,_Burla_et_al.,_1989)
_diffrn_ambient_temperature      294
_diffrn_measurement_details
;
  15403 reflections were collected using program Collect
 ("Collect" Data collection software, Nonius B.V., 1998)
 The conditions were as follow : crystal to detector distance =  35. mm.
 Scan angle =  2.0 deg 1 scans of  260 sec per frame.
 Data collection was divided into  2 set(s)
 with the following starting angles and number of frames :

 Set 1 Theta =    5.90 Omega =    0.00 Kappa =    0.00  113 frames
 Set 2 Theta =   -4.40 Kappa =  136.00 Phi   =    0.00   16 frames
 Friedel pairs were averaged. Internal R = 0.08
;
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.080
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            15403
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.557
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.33
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             3184
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.764
_refine_diff_density_min         -0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   12.264
_refine_ls_goodness_of_fit_ref   1.538
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     496
_refine_ls_number_reflns         2748
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.276
_refine_ls_R_factor_gt           0.065
_refine_ls_shift/esd_mean        0.001
_refine_ls_shift/su_max          0.013
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.422
_refine_ls_wR_factor_ref         0.086
_reflns_number_gt                2748
_reflns_number_total             9161
_reflns_threshold_expression     >3.0\s(I)
_cod_data_source_file            ic001205b_3.cif
_cod_data_source_block           st712
_cod_original_cell_volume        7591(1)
_cod_database_code               4319852