Chromophoric dipyrrin complexes capable of binding to TiO2: synthesis, structure and spectroscopy.
Hall, Jeremy D.; McLean, Tracey M.; Smalley, Serena J.; Waterland, Mark R.; Telfer, Shane G.; Dalton transactions (Cambridge, England : 2003) 39 (2010) 437–445; doi:10.1039/b912332f

data_7024187
_publ_section_title
;
 Chromophoric dipyrrin complexes capable of binding to TiO2: synthesis,
 structure and spectroscopy.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              437
_journal_page_last               445
_journal_paper_doi               10.1039/b912332f
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         0.5(C48H33RhN6O6)
_chemical_formula_sum            'C48 H37 N6 O8 Rh'
_chemical_formula_weight         928.75
_chemical_name_systematic
;
?
;
_space_group_IT_number           73
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-I 2b 2c'
_symmetry_space_group_name_H-M   'I b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.5452(8)
_cell_length_b                   16.1898(9)
_cell_length_c                   40.0972(11)
_cell_measurement_reflns_used    255
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      137.81
_cell_measurement_theta_min      26.11
_cell_volume                     8793.1(8)
_computing_cell_refinement       'FSProcess in Process-Auto (Rigaku, 1998)'
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'FSProcess in Process-Auto (Rigaku, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.872
_diffrn_measured_fraction_theta_max 0.872
_diffrn_measurement_device_type  'Rigaku Spider'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  'Rigaku VariMax-HF Confocal Optical System'
_diffrn_radiation_source         'Rigaku MM007 rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3770
_diffrn_reflns_theta_full        71.93
_diffrn_reflns_theta_max         71.93
_diffrn_reflns_theta_min         6.54
_exptl_absorpt_coefficient_mu    3.649
_exptl_absorpt_correction_T_max  0.9644
_exptl_absorpt_correction_T_min  0.5289
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3808
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
The final R factor was obtained after implementing
the squeeze routine in Platon to account for
severely disordered solvent H2O molecules,
which appeared to be H-bonded to one of the carboxyl
groups (O3). A void space of 1301 \%A3
was calculated (15% of the unit cell volume) along an
electron count per cell of 158. This corresponds
almost exactly to 16 H2O molecules per unit cell
hence the molecular weight, density and F000
were calculated using the formula C48H33RhN6O6?2H2O.
;
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         3770
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+62.4156P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1649
_refine_ls_wR_factor_ref         0.1714
_reflns_number_gt                2806
_reflns_number_total             3770
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b912332f.txt
_cod_data_source_block           '[Rh(Lb)3]'
_cod_original_sg_symbol_H-M      Ibca
_cod_database_code               7024187