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_7038088
_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         'C20 H18 N4 O3 Re'
_chemical_formula_sum            'C20 H19 N4 O3 Re'
_chemical_formula_weight         549.59
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-09-05
_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                92.481(5)
_cell_angle_beta                 105.021(5)
_cell_angle_gamma                104.660(5)
_cell_formula_units_Z            4
_cell_length_a                   9.168(5)
_cell_length_b                   15.214(5)
_cell_length_c                   15.358(5)
_cell_measurement_reflns_used    15455
_cell_measurement_temperature    293
_cell_measurement_theta_max      71.8
_cell_measurement_theta_min      6.6
_cell_volume                     1988.0(14)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 rc14 (Rigaku, 2009)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 rc14 (Rigaku, 2009)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 rc14 (Rigaku, 2009)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector                 RX
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_details
;
scan:
    Number of images: 36
               Slice: 20.0000 - 200.0000
         Image width: 5.0000
            Exp time: 120.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 0.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 36
               Slice: 20.0000 - 200.0000
         Image width: 5.0000
            Exp time: 120.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 270.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 36
               Slice: 20.0000 - 200.0000
         Image width: 5.0000
            Exp time: 120.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 0.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 35
               Slice: 22.0000 - 197.0000
         Image width: 5.0000
            Exp time: 120.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 270.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 35
               Slice: 21.0000 - 196.0000
         Image width: 5.0000
            Exp time: 120.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 180.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 34
               Slice: 25.0000 - 195.0000
         Image width: 5.0000
            Exp time: 120.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 90.0000
                 XTD: 127.4000
              2theta: 0.0000
;
_diffrn_measurement_device
;
Crystal Goniometer
;
_diffrn_measurement_device_type  'Rigaku Spider'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       FS_PROCESS
_diffrn_orient_matrix_UB_11      -0.009848
_diffrn_orient_matrix_UB_12      -0.066976
_diffrn_orient_matrix_UB_13      -0.008836
_diffrn_orient_matrix_UB_21      -0.002124
_diffrn_orient_matrix_UB_22      -0.004739
_diffrn_orient_matrix_UB_23      0.064426
_diffrn_orient_matrix_UB_31      -0.116990
_diffrn_orient_matrix_UB_32      -0.013083
_diffrn_orient_matrix_UB_33      -0.019468
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_laue_measured_fraction_full 0.980
_diffrn_reflns_laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27861
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        71.8
_diffrn_reflns_theta_max         71.8
_diffrn_reflns_theta_min         6.6
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    11.802
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.456
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.836
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.409
_refine_diff_density_min         -2.189
_refine_diff_density_rms         0.212
_refine_ls_extinction_coef       0.0014(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         7422
_refine_ls_number_restraints     266
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0409P)^2^+24.7942P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1374
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6551
_reflns_number_total             7422
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04466a2.cif
_cod_data_source_block           c6
_cod_depositor_comments
'Adding full bibliography for 7038083--7038090.cif.'
_cod_database_code               7038088
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C27-C26A = C28B-C27 = C28A-C27 = C27-C26B
 1.54 with sigma of 0.02
 C1A1-C127 = C2A1-C127
 1.54 with sigma of 0.02
 H1BA-H2AA
 -2 with sigma of 0.02
 H112_$1-H28D_$2
 -2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N114 \\sim C115 \\sim C116 \\sim C117 \\sim C118 \\sim C119 \\sim C120 \\sim
C121 \\sim C122 \\sim C123 \\sim N124 \\sim Re10: within 1.7A with sigma of
0.005 and sigma for terminal atoms of 0.02
N24 \\sim C23 \\sim C22 \\sim C21 \\sim C20 \\sim C19 \\sim C18 \\sim C17 \\sim
C16 \\sim C15 \\sim N14 \\sim Re1: within 1.7A with sigma of 0.005 and sigma
for terminal atoms of 0.02
C19 \\sim N25 \\sim C26A \\sim C27 \\sim C28A: within 1.7A with sigma of 0.01
and sigma for terminal atoms of 0.02
N8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C127) = Uanis(C27)
Uanis(C1A1) = Uanis(C26A)
Uanis(C28B) = Uanis(C28A)
Uanis(C26A) = Uanis(C26B)
Uanis(C1B1) = Uanis(C1A1)
4. Rigid body (RIGU) restrains
 Re1, C6, O7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Re1, C4, O5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Re1, C0AA, O3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Re10, C102, O103
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Re10, C106, O107
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Re10, C104, O105
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C26B)=Sof(H26C)=Sof(H26D)=Sof(H27C)=Sof(H27D)=Sof(C28B)=Sof(H28D)=
 Sof(H28E)=Sof(H28F)=1-FVAR(1)
 Sof(C26A)=Sof(H26A)=Sof(H26B)=Sof(H27A)=Sof(H27B)=Sof(C28A)=Sof(H28A)=
 Sof(H28B)=Sof(H28C)=FVAR(1)
 Sof(H12A)=Sof(H12B)=Sof(C1B1)=Sof(H1BA)=Sof(H1BB)=1-FVAR(2)
 Sof(C1A1)=Sof(H1AA)=Sof(H1AB)=Sof(H12C)=Sof(H12D)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C1A1(H1AA,H1AB), C127(H12C,H12D), C127(H12A,H12B), C26A(H26A,H26B), C26B(H26C,
 H26D), C27(H27A,H27B), C27(H27C,H27D), C1B1(H1BA,H1BB)
6.b Aromatic/amide H refined with riding coordinates:
 C123(H123), C17(H17), C110(H110), C113(H113), C116(H116), C109(H109), C9(H9),
 C23(H23), C12(H12), C16(H16), C13(H13), C11(H11), C10(H10), C121(H121),
 C21(H21), C112(H112), C111(H111), C122(H122), C15(H15), C115(H115), C117(H117),
  C22(H22)
6.c Idealised Me refined as rotating group:
 C2A1(H2AA,H2AB,H2AC), C28A(H28A,H28B,H28C), C28B(H28D,H28E,H28F)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'