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_7038085
_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         'C30 H21 N2 O3 P Re S'
_chemical_formula_sum            'C30 H21 N2 O3 P Re S'
_chemical_formula_weight         706.72
_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
_audit_creation_date             2015-09-08
_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                110.002(8)
_cell_angle_beta                 99.723(7)
_cell_angle_gamma                102.301(7)
_cell_formula_units_Z            4
_cell_length_a                   11.6593(2)
_cell_length_b                   14.0709(3)
_cell_length_c                   18.5868(13)
_cell_measurement_reflns_used    5218
_cell_measurement_temperature    123
_cell_measurement_theta_max      71.9
_cell_measurement_theta_min      6.7
_cell_volume                     2700.8(3)
_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)'
_diffrn_ambient_temperature      123
_diffrn_detector                 RX
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details
;
scan:
    Number of images: 36
               Slice: 20.0000 - 200.0000
         Image width: 5.0000
            Exp time: 60.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 0.0000
                 XTD: 127.4000
              2theta: 0.0411
scan:
    Number of images: 36
               Slice: 20.0000 - 200.0000
         Image width: 5.0000
            Exp time: 60.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 90.0000
                 XTD: 127.4000
              2theta: 0.0411
scan:
    Number of images: 36
               Slice: 20.0000 - 200.0000
         Image width: 5.0000
            Exp time: 60.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 0.0000
                 XTD: 127.4000
              2theta: 0.0411
scan:
    Number of images: 35
               Slice: 21.0000 - 196.0000
         Image width: 5.0000
            Exp time: 60.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 90.0000
                 XTD: 127.4000
              2theta: 0.0411
scan:
    Number of images: 34
               Slice: 20.0000 - 190.0000
         Image width: 5.0000
            Exp time: 60.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 180.0000
                 XTD: 127.4000
              2theta: 0.0411
scan:
    Number of images: 33
               Slice: 24.0000 - 189.0000
         Image width: 5.0000
            Exp time: 60.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 270.0000
                 XTD: 127.4000
              2theta: 0.0411
;
_diffrn_measurement_device
;
Crystal Goniometer
;
_diffrn_measurement_device_type
;
Rigaku RAXIS conversion
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       FS_PROCESS
_diffrn_orient_matrix_UB_11      -0.085956
_diffrn_orient_matrix_UB_12      0.002792
_diffrn_orient_matrix_UB_13      -0.006238
_diffrn_orient_matrix_UB_21      0.029798
_diffrn_orient_matrix_UB_22      0.078933
_diffrn_orient_matrix_UB_23      0.026280
_diffrn_orient_matrix_UB_31      -0.001944
_diffrn_orient_matrix_UB_32      0.004056
_diffrn_orient_matrix_UB_33      -0.052847
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0742
_diffrn_reflns_av_unetI/netI     0.0785
_diffrn_reflns_laue_measured_fraction_full 0.983
_diffrn_reflns_laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            36264
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        65.083
_diffrn_reflns_theta_max         65.083
_diffrn_reflns_theta_min         6.675
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    10.370
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.273
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1380
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.14
_refine_diff_density_max         5.278
_refine_diff_density_min         -5.116
_refine_diff_density_rms         0.284
_refine_ls_extinction_coef       0.00016(6)
_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   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         9067
_refine_ls_number_restraints     330
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0686
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1128P)^2^+27.5553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1757
_refine_ls_wR_factor_ref         0.2189
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7437
_reflns_number_total             9067
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04466a2.cif
_cod_data_source_block           c3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7038083--7038090.cif.
;
_cod_database_code               7038085
_shelx_estimated_absorpt_t_max   0.325
_shelx_estimated_absorpt_t_min   0.063
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
C9B \\sim C8B \\sim C7B \\sim C6B \\sim N2B \\sim C5B \\sim C4B \\sim C3B \\sim
C2B \\sim C1B \\sim N1B: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
H9A \\sim C20B \\sim C21B \\sim C16B \\sim C19B \\sim C18B \\sim C17B: within
1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
C20A \\sim C15A \\sim C16A \\sim C17A \\sim C18A \\sim C19A: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.04
C5A \\sim C6A \\sim C7A \\sim C8A \\sim C9A \\sim N2A \\sim C4A \\sim N1A \\sim
C1A \\sim C2A \\sim C3A: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.04
Uanis(O3A) \\sim Ueq, Uanis(O1A) \\sim Ueq, Uanis(O2A) \\sim Ueq, Uanis(O2B)
\\sim Ueq, Uanis(O1B) \\sim Ueq, Uanis(O3B) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(N1A) \\sim Ueq, Uanis(N2A) \\sim Ueq, Uanis(N1B) \\sim Ueq, Uanis(N2B)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C20) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C21) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C19B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C3B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C21B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C3A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C12A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C15A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C21) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Aromatic/amide H refined with riding coordinates:
 C8B(H8B), C25B(H25B), C27B(H27B), C18B(H18B), C17B(H17B), C2B(H2B),
 C26B(H26B), C19A(H19A), C23B(H23B), C18A(H18A), C20A(H20A), C19B(H19B),
 C12B(H12B), C17A(H17A), C1A(H1A), C1B(H1B), C22A(H22A), C9B(H9B), C3B(H3B),
 C23A(H23A), C24B(H24B), C2A(H2A), C8A(H8A), C055(H055), C13A(H13A), C11B(H11B),
  C21B(H21B), C20B(H20B), C26A(H26A), C3A(H3A), C7A(H7A), C13B(H13B),
 C14B(H14B), C14A(H14A), C16A(H16A), C7B(H7B), C15B(H15B), C24A(H24A),
 C11A(H11A), C25A(H25A), C12A(H12A), C9A(H9A)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'