Structural isolation of NIR absorbing ferrocenyl bridged N-confused fused expanded phlorin, N-confused porphodimethene and the π-extended corrorin isomer: synthesis and characterization
Chakraborty, Buddhadeb; Sahoo, Sumit; Narayansamy, Raja; Usharani, Dandamudi; Rath, Harapriya; Dalton Transactions  (2021) –; doi:10.1039/D1DT02385C

data_7708433
_publ_section_title
;
 Structural isolation of NIR absorbing ferrocenyl bridged N-confused fused
 expanded phlorin, N-confused porphodimethene and the \p-extended corrorin
 isomer: synthesis and characterization
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02385C
_journal_year                    2021
_chemical_formula_moiety         'C68 H40 F8 Fe N4'
_chemical_formula_sum            'C68 H40 F8 Fe N4'
_chemical_formula_weight         1120.89
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2021-08-16
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2021-08-17 deposited with the CCDC.	2021-09-07 downloaded from the CCDC.
;
_cell_angle_alpha                118.145(5)
_cell_angle_beta                 93.156(5)
_cell_angle_gamma                99.868(5)
_cell_formula_units_Z            2
_cell_length_a                   10.8521(18)
_cell_length_b                   17.560(3)
_cell_length_c                   17.760(3)
_cell_measurement_reflns_used    7512
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.99
_cell_measurement_theta_min      2.30
_cell_volume                     2903.9(9)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.73
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0821
_diffrn_reflns_av_unetI/netI     0.1092
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_number            10092
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.272
_exptl_absorpt_coefficient_mu    0.330
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_description       block
_exptl_crystal_F_000             1148
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     734
_refine_ls_number_reflns         10092
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1055
_refine_ls_R_factor_gt           0.0735
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0839P)^2^+3.3586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1804
_refine_ls_wR_factor_ref         0.1910
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6742
_reflns_number_total             10092
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02385c2.cif
_cod_data_source_block           mo_hr140120_0m_a
_cod_original_cell_volume        2903.9(8)
_cod_database_code               7708433
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C00J(H00J)
2.b Secondary CH2 refined with riding coordinates:
 C01K(H01B,H01D)
2.c Aromatic/amide H refined with riding coordinates:
 C00T(H00T), C00V(H00V), C00Y(H00Y), C010(H010), C011(H011), C012(H012),
 C014(H014), C016(H016), C018(H018), C01A(H01A), C01C(H01C), C01E(H01E),
 C01G(H01G), C01H(H01H), C01I(H01I), C01J(H01J), C01L(H01L), C01M(H01M),
 C01N(H01N), C01O(H01O), C01P(H01P), C01Q(H01Q), C01V(H01V), C01W(H01W),
 C01X(H01X), C01Z(H01Z), C020(H020), C021(H021), C022(H022), C023(H023),
 C024(H024), C025(H025), C026(H026), C027(H027), C028(H028), C029(H029)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'