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_7038084
_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_sum            'C51 H36 N2 O6 P2 Re2 S'
_chemical_formula_weight         1239.22
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-09-09 deposited with the CCDC.
2016-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.534(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9320(2)
_cell_length_b                   17.1113(3)
_cell_length_c                   24.1889(17)
_cell_measurement_reflns_used    36007
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      71.9
_cell_measurement_theta_min      6.6
_cell_volume                     4523.2(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    '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      133(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Rigaku Spider'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1052
_diffrn_reflns_av_unetI/netI     0.0887
_diffrn_reflns_laue_measured_fraction_full 0.989
_diffrn_reflns_laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            49283
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.115
_diffrn_reflns_theta_min         6.571
_diffrn_source                   'Rigaku MM007 rotating anode'
_exptl_absorpt_coefficient_mu    11.842
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.365
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.374
_refine_diff_density_min         -2.931
_refine_diff_density_rms         0.215
_refine_ls_extinction_coef       0.000200(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         8654
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+46.9301P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1110
_refine_ls_wR_factor_ref         0.1186
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7922
_reflns_number_total             8654
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04466a2.cif
_cod_data_source_block           c2
_cod_depositor_comments
;
Adding full bibliography for 7038083--7038090.cif.

2018-01-25
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         619.61
_cod_original_formula_units_Z            8
_cod_original_formula_sum        'C25.50 H18 N O3 P Re S0.50'
_cod_database_code               7038084
_shelx_estimated_absorpt_t_min   0.059
_shelx_estimated_absorpt_t_max   0.384
_shelxl_version_number           2013-2
_shelx_res_checksum              25551