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_7036444
_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         'C10 H11 Cl N3 O3 Re, 0.8(C4 H8 O)'
_chemical_formula_sum            'C13.2 H17.4 Cl N3 O3.8 Re'
_chemical_formula_weight         500.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-09-02
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 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                90
_cell_angle_beta                 110.011(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7779(11)
_cell_length_b                   16.2401(12)
_cell_length_c                   10.3889(9)
_cell_measurement_reflns_used    2600
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.4210
_cell_measurement_theta_min      3.2590
_cell_volume                     1867.2(3)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)'
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)'
_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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.805
_diffrn_measurement_details
;
  1 omega    8.00   72.00   1.0000   20.8850
omega____ theta____ kappa____ phi______ frames
    -        9.8631   37.0000 -180.0000 64

  2 omega  -54.00   30.00   1.0000   20.8850
omega____ theta____ kappa____ phi______ frames
    -        9.8631  -77.0000   60.0000 84
;
_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      -0.0555707000
_diffrn_orient_matrix_UB_12      0.0155837000
_diffrn_orient_matrix_UB_13      0.0022166000
_diffrn_orient_matrix_UB_21      0.0103933000
_diffrn_orient_matrix_UB_22      0.0376436000
_diffrn_orient_matrix_UB_23      -0.0287211000
_diffrn_orient_matrix_UB_31      -0.0301076000
_diffrn_orient_matrix_UB_32      -0.0157780000
_diffrn_orient_matrix_UB_33      -0.0666530000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0799
_diffrn_reflns_av_unetI/netI     0.1055
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.805
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7163
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.805
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.925
_diffrn_reflns_theta_min         2.434
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.670
_exptl_absorpt_correction_T_max  0.582
_exptl_absorpt_correction_T_min  0.100
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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_colour_primary    yellow
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_description       prism
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.6978
_exptl_crystal_size_mid          0.1868
_exptl_crystal_size_min          0.064
_refine_diff_density_max         2.132
_refine_diff_density_min         -3.302
_refine_diff_density_rms         0.277
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         3966
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.1388
_refine_ls_R_factor_gt           0.0887
_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^)+(0.1708P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2417
_refine_ls_wR_factor_ref         0.3216
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2137
_reflns_number_total             3966
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02793d2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7036443--7036445.cif.'
_cod_original_formula_sum        'C13.20 H17.40 Cl N3 O3.80 Re'
_cod_database_code               7036444
_shelxl_version_number           2013-3
_reflns_odcompleteness_completeness 95.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 O91, C91, C92, C93, C94
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Re1, C1, O1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Re1, C2, O2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Re1, C3, O3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
O91 \\sim C91 \\sim C92 \\sim C93 \\sim C94: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
Re1 \\sim C1 \\sim O1: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Re1 \\sim C2 \\sim O2: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Re1 \\sim C3 \\sim O3: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
4. Others
 Fixed Sof: O91(0.8) C94(0.8) H94A(0.8) H94B(0.8) C93(0.8) H93A(0.8) H93B(0.8)
 C92(0.8) H92A(0.8) H92B(0.8) C91(0.8) H91A(0.8) H91B(0.8)
5.a Free rotating group:
 O91(C94,C93,C92,C91)
5.b Secondary CH2 refined with riding coordinates:
 C94(H94A,H94B), C93(H93A,H93B), C92(H92A,H92B), C91(H91A,H91B)
5.c Aromatic/amide H refined with riding coordinates:
 C12(H12), N3(H3)
5.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              78351
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'