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_4319851
_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
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_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         'C49 H40 Cl2 N4 Ni O2'
_chemical_formula_sum            'C49 H40 Cl2 N4 Ni O2'
_chemical_formula_weight         846.51
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                66.612(8)
_cell_angle_beta                 71.521(8)
_cell_angle_gamma                79.266(8)
_cell_formula_units_Z            2
_cell_length_a                   12.384(1)
_cell_length_b                   13.484(1)
_cell_length_c                   14.285(1)
_cell_measurement_temperature    173
_cell_volume                     2071.5(3)
_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      173
_diffrn_measurement_details
;
  22739 reflections were collected using program Collect
 ("Collect" Data collection software, Nonius B.V., 1998)
 The conditions were as follow : crystal to detector distance =  36. mm.
 Scan angle =  2.0 deg 1 scans of  120 sec per frame.
 Data collection was divided into  4 set(s)
 with the following starting angles and number of frames :

 Set 1 Theta =    8.50 Omega =  180.00 Kappa =    0.00   91 frames
 Set 2 Theta =   -8.20 Kappa =  174.00 Phi   =    0.00   34 frames
 Set 3 Theta =    6.50 Kappa =   67.00 Phi   =    0.00   55 frames
 Set 4 Theta =   -6.10 Kappa = -159.00 Phi   =    0.00   18 frames
 Friedel pairs were averaged. Internal R = 0.04
;
_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  0.040
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22739
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.643
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.36
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.732
_refine_diff_density_min         -0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.747
_refine_ls_goodness_of_fit_ref   1.245
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     523
_refine_ls_number_reflns         6751
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.105
_refine_ls_R_factor_gt           0.070
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.003
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 4Fo^2^/(\s^2^(Fo^2^)+0.0004 Fo^4^)+4.0'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.114
_refine_ls_wR_factor_ref         0.081
_reflns_number_gt                6751
_reflns_number_total             9479
_reflns_threshold_expression     >3.0\s(I)
_cod_data_source_file            ic001205b_2.cif
_cod_data_source_block           st498
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '4Fo^2^/(\s^2^(Fo^2^)+0.0004
Fo^4^)+4.0' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 4Fo^2^/(\s^2^(Fo^2^)+0.0004 Fo^4^)+4.0'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        2071.5(2)
_cod_database_code               4319851