Postcomplexation synthetic routes to dipyrrin complexes.
Perl, David; Bisset, Sean W.; Telfer, Shane G.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 2440–2443; doi:10.1039/c5dt04466a

data_7038087
_publ_section_title
;
 Postcomplexation synthetic routes to dipyrrin complexes.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2440
_journal_page_last               2443
_journal_paper_doi               10.1039/c5dt04466a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C18 H14 N3 O3 Re S'
_chemical_formula_sum            'C18 H14 N3 O3 Re S'
_chemical_formula_weight         538.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-08-31
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_audit_update_record
;
2015-09-09 deposited with the CCDC.
2016-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.575(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.2808(3)
_cell_length_b                   14.7769(3)
_cell_length_c                   16.6692(12)
_cell_measurement_reflns_used    21785
_cell_measurement_temperature    293
_cell_measurement_theta_max      72.0
_cell_measurement_theta_min      6.5
_cell_volume                     3754.5(3)
_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_molecular_graphics
'OLEX (Dolomanov, 2003) and SXGRAPH in WinGX v2013.1'
_computing_publication_material  'SHELXL-13 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      293
_diffrn_detector                 RX
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.9775
_diffrn_measured_fraction_theta_max 0.9775
_diffrn_measurement_details
;
scan:
    Number of images: 64
               Slice: 24.0000 - 184.0000
         Image width: 2.5000
            Exp time: 60.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 0.0000
                 XTD: 127.4000
              2theta: -0.1538
scan:
    Number of images: 54
               Slice: 53.0000 - 188.0000
         Image width: 2.5000
            Exp time: 60.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 270.0000
                 XTD: 127.4000
              2theta: -0.1538
scan:
    Number of images: 72
               Slice: 20.0000 - 200.0000
         Image width: 2.5000
            Exp time: 60.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 180.0000
                 XTD: 127.4000
              2theta: -0.1538
scan:
    Number of images: 60
               Slice: 20.0000 - 170.0000
         Image width: 2.5000
            Exp time: 60.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 270.0000
                 XTD: 127.4000
              2theta: -0.1538
scan:
    Number of images: 68
               Slice: 21.0000 - 191.0000
         Image width: 2.5000
            Exp time: 60.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 90.0000
                 XTD: 127.4000
              2theta: -0.1538
;
_diffrn_measurement_device
;
Crystal Goniometer
;
_diffrn_measurement_device_type  'Rigaku Spider'
_diffrn_measurement_method       \w-scans
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       FS_PROCESS
_diffrn_orient_matrix_UB_11      -0.040889
_diffrn_orient_matrix_UB_12      -0.028965
_diffrn_orient_matrix_UB_13      -0.053299
_diffrn_orient_matrix_UB_21      -0.041357
_diffrn_orient_matrix_UB_22      0.052126
_diffrn_orient_matrix_UB_23      -0.008403
_diffrn_orient_matrix_UB_31      0.030363
_diffrn_orient_matrix_UB_32      0.031993
_diffrn_orient_matrix_UB_33      -0.034564
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            38685
_diffrn_reflns_theta_full        72.0462
_diffrn_reflns_theta_max         72.05
_diffrn_reflns_theta_min         6.54
_diffrn_source                   'Rigaku MM007 rotating anode'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    13.900
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.495
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.9056
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rod
_exptl_crystal_F_000             2033.7019
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.2596
_refine_diff_density_min         -0.8702
_refine_diff_density_rms         0.1142
_refine_ls_d_res_high            0.8103
_refine_ls_d_res_low             6.7734
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0271
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    62
_refine_ls_number_parameters     489
_refine_ls_number_reflns         7223
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.0244
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+5.4051P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0793
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              18
_reflns_limit_h_min              -20
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                6362
_reflns_number_total             7223
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c5dt04466a2.cif
_cod_data_source_block           c5
_cod_depositor_comments
'Adding full bibliography for 7038083--7038090.cif.'
_cod_original_cell_volume        3754.5(4)
_cod_database_code               7038087
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C126 \\sim C127 \\sim C27 \\sim C26 \\sim S25 \\sim S125 \\sim C19 \\sim C119:
within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
3. Others
 Sof(C27)=Sof(H27a)=Sof(H27b)=Sof(H27c)=1-FVAR(1)
 Sof(C26)=Sof(H26a)=Sof(H26b)=Sof(H26c)=FVAR(1)
 Sof(C127)=Sof(H12a)=Sof(H12b)=Sof(H12c)=1-FVAR(2)
 Sof(C126)=Sof(H12d)=Sof(H12e)=Sof(H12f)=FVAR(2)
4.a Me refined with riding coordinates:
 C26(H26a,H26b,H26c), C127(H12a,H12b,H12c), C126(H12d,H12e,H12f), C27(H27a,
 H27b,H27c)
4.b Aromatic/amide H refined with riding coordinates:
 C115(H115), C23(H23), C22(H22), C123(H123), C17(H17), C15(H15), C121(H121),
 C122(H122), C116(H116), C117(H117), C13(H13), C109(H109), C113(H113),
 C110(H110), C111(H111), C9(H9), C11(H11), C12(H12), C10(H10), C16(H16),
 C21(H21), C112(H112)
;
_olex2_submission_special_instructions 'No special instructions were received'