Blue rhenium tricarbonyl DPPZ complexes - low energy charge-transfer absorption at tissue-penetrating wavelengths.
Coogan, M. P.; Platts, J. A.; Chemical communications (Cambridge, England) 52 (2016) 12498–12501; doi:10.1039/c6cc07125b

data_7125143
_publ_section_title
;
 Blue rhenium tricarbonyl DPPZ complexes - low energy charge-transfer
 absorption at tissue-penetrating wavelengths.
;
_journal_issue                   84
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12498
_journal_page_last               12501
_journal_paper_doi               10.1039/c6cc07125b
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C10.5 H5 Br0.5 Mn0.5 N2 O1.5'
_chemical_formula_sum            'C10.5 H6 Br0.5 Mn0.5 N2 O2'
_chemical_formula_weight         259.60
_chemical_name_common            MnBrCO3dppz
_chemical_name_systematic        MnBrCO3dppz
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-08
_audit_creation_method
;
Olex2 1.2-ac21
(compiled 2015.09.16 svn.r134, GUI svn.r4998)
;
_audit_update_record
;
2016-08-22 deposited with the CCDC.
2016-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.067(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.4756(5)
_cell_length_b                   12.4761(3)
_cell_length_c                   7.29758(16)
_cell_measurement_reflns_used    5605
_cell_measurement_temperature    292.78(10)
_cell_measurement_theta_max      77.0350
_cell_measurement_theta_min      3.7780
_cell_volume                     2121.11(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      292.78(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2303
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -110.00 -18.00   1.00    1.00    --  -38.50 -38.00-150.00   92
  2  \w    -64.00  30.00   1.00    1.00    --  -38.50  57.00   0.00   94
  3  \w     17.00 111.00   1.00    1.00    --   42.14  57.00-150.00   94
  4  \w     23.00  96.00   1.00    1.00    --   42.14-125.00 -90.00   73
  5  \w    100.00 178.00   1.00    1.64    --  111.00 111.00 -30.00   78
  6  \w     71.00 178.00   1.00    1.64    --  111.00  15.00 -60.00  107
  7  \w    100.00 178.00   1.00    1.64    --  111.00 111.00  60.00   78
  8  \w    100.00 178.00   1.00    1.64    --  111.00 111.00 150.00   78
  9  \w     99.00 178.00   1.00    1.64    --  111.00  88.00 -74.00   79
 10  \w     40.00 141.00   1.00    1.64    --  111.00 -77.00-180.00  101
 11  \w     31.00 109.00   1.00    1.64    --  111.00 -94.00  60.00   78
 12  \w     41.00 133.00   1.00    1.64    --  111.00 -45.00 150.00   92
 13  \w     85.00 178.00   1.00    1.64    --  111.00  61.00 150.00   93
 14  \w    -29.00  63.00   1.00    1.00    --   42.14 -38.00  60.00   92
 15  \w     17.00 111.00   1.00    1.00    --   42.14  57.00  30.00   94
 16  \w     17.00 111.00   1.00    1.00    --   42.14  57.00 120.00   94
 17  \w     81.00 176.00   1.00    1.64    --  111.00  77.00  90.00   95
 18  \w     85.00 178.00   1.00    1.64    --  111.00  61.00-150.00   93
 19  \w     71.00 178.00   1.00    1.64    --  111.00  15.00  60.00  107
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0099969000
_diffrn_orient_matrix_UB_12      0.0753962000
_diffrn_orient_matrix_UB_13      0.1601252000
_diffrn_orient_matrix_UB_21      0.0421614000
_diffrn_orient_matrix_UB_22      0.0813919000
_diffrn_orient_matrix_UB_23      -0.0667219000
_diffrn_orient_matrix_UB_31      -0.0499666000
_diffrn_orient_matrix_UB_32      0.0541268000
_diffrn_orient_matrix_UB_33      -0.1231991000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            11582
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.309
_diffrn_reflns_theta_min         3.795
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.582
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65337
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_description       block
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         2340
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0268
_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^)+(0.0352P)^2^+2.2005P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0717
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2142
_reflns_number_total             2340
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc07125b2.cif
_cod_data_source_block           mc143
_cod_original_formula_sum        'C10.50 H6 Br0.50 Mn0.50 N2 O2'
_cod_database_code               7125143
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C21 H10 N4O3 Br1 Mn1'
_chemical_oxdiff_usercomment     'Mn dppz br 100K'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C11(H11), C10(H10), C16(H16), C17(H17)
;
_shelx_res_checksum              71410
_olex2_date_sample_data_collection 2016-06-08
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.520
_oxdiff_exptl_absorpt_empirical_full_min 0.788