Tuning Electronic Structure, Redox, and Photophysical Properties in Asymmetric NIR-Absorbing Organometallic BODIPYs.
Zatsikha, Yuriy V.; Maligaspe, Eranda; Purchel, Anatolii A.; Didukh, Natalia O.; Wang, Yefeng; Kovtun, Yuriy P.; Blank, David A.; Nemykin, Victor N.; Inorganic chemistry 54 (2015) 7915–7928; doi:10.1021/acs.inorgchem.5b00992

data_4344032
_publ_section_related_literature
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_publ_section_title
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 Tuning Electronic Structure, Redox, and Photophysical Properties in
 Asymmetric NIR-Absorbing Organometallic BODIPYs.
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_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7915
_journal_page_last               7928
_journal_paper_doi               10.1021/acs.inorgchem.5b00992
_journal_volume                  54
_journal_year                    2015
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C40 H35 B1 F2 Fe1 N2 O4'
_chemical_formula_sum            'C40 H35 B F2 Fe N2 O4'
_chemical_formula_weight         712.38
_space_group_IT_number           45
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'I 2 -2c'
_symmetry_space_group_name_H-M   'I b a 2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             15-04-09
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.720(2)
_cell_length_b                   48.938(7)
_cell_length_c                   8.0507(9)
_cell_measurement_reflns_used    23302
_cell_measurement_temperature    123
_cell_measurement_theta_max      24
_cell_measurement_theta_min      4
_cell_volume                     7375.4(16)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      123
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.259
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       54
_diffrn_reflns_limit_k_min       -54
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            23302
_diffrn_reflns_theta_full        17.441
_diffrn_reflns_theta_max         23.254
_diffrn_reflns_theta_min         3.110
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_time  2
_diffrn_standards_number         23302
_exptl_absorpt_coefficient_mu    0.461
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.40
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2960
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.16
_refine_diff_density_min         -0.96
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9932
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4454
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.2338
_refine_ls_R_factor_gt           0.1118
_refine_ls_shift/su_max          0.0221160
_refine_ls_shift/su_mean         0.0013747
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 34.8 42.0 13.0 
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_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2705
_refine_ls_wR_factor_gt          0.1552
_refine_ls_wR_factor_ref         0.2346
_reflns_limit_h_max              20
_reflns_limit_h_min              0
_reflns_limit_k_max              54
_reflns_limit_k_min              0
_reflns_limit_l_max              8
_reflns_limit_l_min              -8
_reflns_number_gt                1804
_reflns_number_total             4991
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.2180
_oxford_refine_ls_scale          0.12668(13)
_oxford_reflns_number_all        4968
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title MonoFcBODIPY
_cod_data_source_file            ic5b00992_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4344032--4344035.cif.'
_cod_original_cell_volume        7375.4(15)
_cod_original_sg_symbol_H-M      'I b a 2 '
_cod_original_formula_sum        'C40 H35 B1 F2 Fe1 N2 O4'
_cod_database_code               4344032
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
EQUIVALENCE C(1,U[11]) UNTIL C(5) 
EQUIVALENCE C(1,U[22]) UNTIL C(5) 
EQUIVALENCE C(1,U[33]) UNTIL C(5) 
EQUIVALENCE C(1,U[12]) UNTIL C(5) 
EQUIVALENCE C(1,U[13]) UNTIL C(5) 
EQUIVALENCE C(1,U[23]) UNTIL C(5) 
EQUIVALENCE C(6,U[11]) UNTIL C(10) 
EQUIVALENCE C(6,U[22]) UNTIL C(10) 
EQUIVALENCE C(6,U[33]) UNTIL C(10) 
EQUIVALENCE C(6,U[12]) UNTIL C(10) 
EQUIVALENCE C(6,U[13]) UNTIL C(10) 
EQUIVALENCE C(6,U[23]) UNTIL C(10) 
EQUIVALENCE C(20,U[11]) UNTIL C(25) 
EQUIVALENCE C(20,U[22]) UNTIL C(25) 
EQUIVALENCE C(20,U[33]) UNTIL C(25) 
EQUIVALENCE C(20,U[12]) UNTIL C(25) 
EQUIVALENCE C(20,U[13]) UNTIL C(25) 
EQUIVALENCE C(20,U[23]) UNTIL C(25) 
EQUIVALENCE C(27,U[11]) UNTIL C(30) 
EQUIVALENCE C(27,U[22]) UNTIL C(30) 
EQUIVALENCE C(27,U[33]) UNTIL C(30) 
EQUIVALENCE C(27,U[12]) UNTIL C(30) 
EQUIVALENCE C(27,U[13]) UNTIL C(30) 
EQUIVALENCE C(27,U[23]) UNTIL C(30) 
EQUIVALENCE C(15,U[11]) C(16,U[11]) C(35,U[11]) C(37,U[11]) C(38,U[11]) 
EQUIVALENCE C(15,U[22]) C(16,U[22]) C(35,U[22]) C(37,U[22]) C(38,U[22]) 
EQUIVALENCE C(15,U[33]) C(16,U[33]) C(35,U[33]) C(37,U[33]) C(38,U[33]) 
EQUIVALENCE C(15,U[12]) C(16,U[12]) C(35,U[12]) C(37,U[12]) C(38,U[12]) 
EQUIVALENCE C(15,U[13]) C(16,U[13]) C(35,U[13]) C(37,U[13]) C(38,U[13]) 
EQUIVALENCE C(15,U[23]) C(16,U[23]) C(35,U[23]) C(37,U[23]) C(38,U[23]) 
EQUIVALENCE C(17,U[11]) C(31,U[11]) 
EQUIVALENCE C(17,U[22]) C(31,U[22]) 
EQUIVALENCE C(17,U[33]) C(31,U[33]) 
EQUIVALENCE C(17,U[12]) C(31,U[12]) 
EQUIVALENCE C(17,U[13]) C(31,U[13]) 
EQUIVALENCE C(17,U[23]) C(31,U[23]) 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  18,X'S) H   ( 182,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) H   ( 192,X'S) H   ( 193,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  32,X'S) H   ( 322,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 332,X'S) H   ( 331,X'S) H   ( 333,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
RIDE C   (  40,X'S) H   ( 402,X'S) H   ( 401,X'S) H   ( 403,X'S) 
END                                                                             
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_iucr_refine_instruction_details_restraints
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NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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