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_4344034
_publ_section_title
;
 Tuning Electronic Structure, Redox, and Photophysical Properties in
 Asymmetric NIR-Absorbing Organometallic BODIPYs.
;
_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_formula_moiety         'C49 H44 B1 F2 Fe1 N3 O4'
_chemical_formula_sum            'C49 H44 B F2 Fe N3 O4'
_chemical_formula_weight         843.56
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2n'
_symmetry_space_group_name_H-M   'P 1 1 21/n'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                116.998(8)
_cell_formula_units_Z            4
_cell_length_a                   11.2986(2)
_cell_length_b                   11.5422(8)
_cell_length_c                   36.2597(6)
_cell_measurement_reflns_used    23630
_cell_measurement_temperature    123
_cell_measurement_theta_max      27
_cell_measurement_theta_min      4
_cell_volume                     4213.3(4)
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      123
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.993
_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  0.029
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            23630
_diffrn_reflns_theta_full        26.110
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.996
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_time  2
_diffrn_standards_number         23630
_exptl_absorpt_coefficient_mu    0.416
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.110
_refine_diff_density_max         2.41
_refine_diff_density_min         -0.79
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9940
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         9563
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0784
_refine_ls_shift/su_max          0.0007075
_refine_ls_shift/su_mean         0.0000271
_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: 
 30.5 40.8 11.5 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1644
_refine_ls_wR_factor_gt          0.1550
_refine_ls_wR_factor_ref         0.1644
_reflns_limit_h_max              13
_reflns_limit_h_min              -14
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              46
_reflns_limit_l_min              0
_reflns_number_gt                7978
_reflns_number_total             9594
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.34
_oxford_diffrn_Wilson_scale      6.05
_oxford_refine_ls_r_factor_ref   0.0868
_oxford_refine_ls_scale          0.4161(5)
_oxford_reflns_number_all        9563
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_cod_data_source_file            ic5b00992_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 4344032--4344035.cif.'
_cod_original_sg_symbol_H-M      'P 1 1 21/n '
_cod_original_formula_sum        'C49 H44 B1 F2 Fe1 N3 O4'
_cod_database_code               4344034
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (   8,X'S) H   (  21,X'S) 
RIDE C   (   7,X'S) H   (  31,X'S) 
RIDE C   (   6,X'S) H   (  41,X'S) 
RIDE C   (  10,X'S) H   (  51,X'S) 
RIDE C   (   9,X'S) H   (  61,X'S) 
RIDE C   (   2,X'S) H   (  81,X'S) 
RIDE C   (   3,X'S) H   (  91,X'S) 
RIDE C   (   4,X'S) H   ( 101,X'S) 
RIDE C   (   5,X'S) H   ( 111,X'S) 
RIDE C   (  11,X'S) H   ( 121,X'S) 
RIDE C   (  12,X'S) H   ( 131,X'S) 
RIDE C   (  18,X'S) H   ( 211,X'S) H   ( 212,X'S) 
RIDE C   (  19,X'S) H   ( 222,X'S) H   ( 223,X'S) H   ( 221,X'S) 
RIDE C   (  21,X'S) H   ( 251,X'S) 
RIDE C   (  22,X'S) H   ( 261,X'S) 
RIDE C   (  23,X'S) H   ( 271,X'S) 
RIDE C   (  24,X'S) H   ( 281,X'S) 
RIDE C   (  25,X'S) H   ( 291,X'S) 
RIDE C   (  26,X'S) H   ( 301,X'S) 
RIDE C   (  40,X'S) H   ( 371,X'S) 
RIDE C   (  41,X'S) H   ( 381,X'S) 
RIDE C   (  43,X'S) H   ( 401,X'S) 
RIDE C   (  44,X'S) H   ( 411,X'S) 
RIDE C   (  48,X'S) H   ( 441,X'S) H   ( 442,X'S) H   ( 443,X'S) 
RIDE C   (  49,X'S) H   ( 452,X'S) H   ( 453,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) 
RIDE C   (  35,X'S) H   ( 511,X'S) 
RIDE C   (  36,X'S) H   ( 521,X'S) 
RIDE C   (  37,X'S) H   ( 531,X'S) 
RIDE C   (  38,X'S) H   ( 541,X'S) 
RIDE C   (  39,X'S) H   ( 551,X'S) 
RIDE C   (  32,X'S) H   ( 582,X'S) H   ( 581,X'S) 
RIDE C   (  33,X'S) H   ( 592,X'S) H   ( 591,X'S) H   ( 593,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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