Luminescent rhenium(i) tricarbonyl complexes with pyrazolylamidino ligands: photophysical, electrochemical, and computational studies.
Gómez-Iglesias, Patricia; Guyon, Fabrice; Khatyr, Abderrahim; Ulrich, Gilles; Knorr, Michael; Martín-Alvarez, Jose Miguel; Miguel, Daniel; Villafañe, Fernando; Dalton transactions (Cambridge, England : 2003) 44 (2015) 17516–17528; doi:10.1039/c5dt02793d

data_7036443
_publ_section_title
;
 Luminescent rhenium(i) tricarbonyl complexes with pyrazolylamidino
 ligands: photophysical, electrochemical, and computational studies.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17516
_journal_page_last               17528
_journal_paper_doi               10.1039/c5dt02793d
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C8 H7 Cl N3 O3 Re'
_chemical_formula_sum            'C8 H7 Cl N3 O3 Re'
_chemical_formula_weight         414.82
_chemical_name_systematic
;
 ?
;
_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     direct
_audit_creation_date             2015-02-17
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-09-08 deposited with the CCDC.
2015-09-08 downloaded from the CCDC.
;
_cell_angle_alpha                103.633(6)
_cell_angle_beta                 103.439(7)
_cell_angle_gamma                104.924(7)
_cell_formula_units_Z            2
_cell_length_a                   6.5720(6)
_cell_length_b                   9.0667(7)
_cell_length_c                   10.3877(7)
_cell_measurement_reflns_used    1727
_cell_measurement_temperature    566(2)
_cell_measurement_theta_max      74.9690
_cell_measurement_theta_min      4.6080
_cell_volume                     552.20(9)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_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_temperature      566.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_details
;
  1 omega   15.00  113.00   1.0000    1.2250
omega____ theta____ kappa____ phi______ frames
    -       40.9313   57.0000  -30.0000 98

  2 omega   69.00   95.00   1.0000    4.9000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  -30.0000 26

  3 omega   43.00   93.00   1.0000    4.9000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000   60.0000 50

  4 omega   59.00   91.00   1.0000    4.9000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  120.0000 32

  5 omega   47.00   98.00   1.0000    4.9000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000   90.0000 51

  6 omega   39.00  112.00   1.0000    4.9000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -125.0000   60.0000 73

  7 omega   41.00   94.00   1.0000    4.9000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000  -60.0000 53

  8 omega   37.00   77.00   1.0000    4.9000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  -90.0000 40

  9 omega   48.00  109.00   1.0000    4.9000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000 -180.0000 61

 10 omega   36.00   91.00   1.0000    4.9000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000 -180.0000 55

 11 omega   86.00  174.00   1.0000    4.9000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000 -180.0000 88

 12 omega   86.00  171.00   1.0000    4.9000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000   90.0000 85

 13 omega   13.00  117.00   1.0000    1.2250
omega____ theta____ kappa____ phi______ frames
    -       40.9313   77.0000 -150.0000 104

 14 omega    1.00   81.00   1.0000    1.2250
omega____ theta____ kappa____ phi______ frames
    -       40.9313  -99.0000   90.0000 80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.2238531000
_diffrn_orient_matrix_UB_12      0.1377575000
_diffrn_orient_matrix_UB_13      0.0594359000
_diffrn_orient_matrix_UB_21      0.1037460000
_diffrn_orient_matrix_UB_22      -0.1068949000
_diffrn_orient_matrix_UB_23      -0.0833672000
_diffrn_orient_matrix_UB_31      -0.0658267000
_diffrn_orient_matrix_UB_32      0.0625464000
_diffrn_orient_matrix_UB_33      -0.1237725000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0702
_diffrn_reflns_av_unetI/netI     0.0965
_diffrn_reflns_laue_measured_fraction_full 0.983
_diffrn_reflns_laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3085
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.766
_diffrn_reflns_theta_min         4.611
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    23.758
_exptl_absorpt_correction_T_max  0.532
_exptl_absorpt_correction_T_min  0.155
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.495
_exptl_crystal_description       prism
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.2694
_exptl_crystal_size_mid          0.172
_exptl_crystal_size_min          0.0731
_refine_diff_density_max         1.536
_refine_diff_density_min         -1.752
_refine_diff_density_rms         0.294
_refine_ls_extinction_coef       0.0104(6)
_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   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         2158
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0551
_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^)+(0.0389P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1032
_refine_ls_wR_factor_ref         0.1100
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1893
_reflns_number_total             2158
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02793d2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7036443--7036445.cif.'
_cod_original_cell_volume        552.19(8)
_cod_database_code               7036443
_shelxl_version_number           2013-3
_chemical_oxdiff_formula         'C8 H6 Cl1 N3 O3 Re1'
_reflns_odcompleteness_completeness 98.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), N3(H3)
2.b Idealised Me refined as rotating group:
 C22(H22a,H22b,H22c)
;
_shelx_res_checksum              73296
_olex2_submission_special_instructions 'No special instructions were received'