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_7036445
_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         'C15 H13 Br N3 O3 Re, C4 H8 O'
_chemical_formula_sum            'C19 H21 Br N3 O4 Re'
_chemical_formula_weight         621.50
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-08-27
_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                 99.020(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1347(2)
_cell_length_b                   14.0546(4)
_cell_length_c                   19.7121(6)
_cell_measurement_reflns_used    2992
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.7647
_cell_measurement_theta_min      2.5350
_cell_volume                     2225.81(11)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39)'
_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 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.846
_diffrn_measurement_details
;
  1 omega   34.00  123.00   1.0000   10.9600
omega____ theta____ kappa____ phi______ frames
    -       19.5043  179.0000 -180.0000 89

  2 omega  -74.00   27.00   1.0000   10.9600
omega____ theta____ kappa____ phi______ frames
    -       19.5043  -37.0000 -120.0000 101
;
_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      0.0305253000
_diffrn_orient_matrix_UB_12      0.0432854000
_diffrn_orient_matrix_UB_13      0.0156848000
_diffrn_orient_matrix_UB_21      -0.0332257000
_diffrn_orient_matrix_UB_22      0.0251622000
_diffrn_orient_matrix_UB_23      -0.0302312000
_diffrn_orient_matrix_UB_31      -0.0758929000
_diffrn_orient_matrix_UB_32      0.0063933000
_diffrn_orient_matrix_UB_33      0.0129145000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_laue_measured_fraction_full 0.991
_diffrn_reflns_laue_measured_fraction_max 0.846
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7430
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.846
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.750
_diffrn_reflns_theta_min         2.545
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.282
_exptl_absorpt_correction_T_max  0.462
_exptl_absorpt_correction_T_min  0.152
_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_colour_primary    yellow
_exptl_crystal_density_diffrn    1.855
_exptl_crystal_description       plate
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.5843
_exptl_crystal_size_mid          0.1981
_exptl_crystal_size_min          0.1311
_refine_diff_density_max         0.719
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       0.00070(8)
_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   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         4442
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0242P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0633
_refine_ls_wR_factor_ref         0.0727
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3348
_reflns_number_total             4442
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02793d2.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 7036443--7036445.cif.'
_cod_original_cell_volume        2225.83(11)
_cod_database_code               7036445
_reflns_odcompleteness_completeness 94.33
_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
 O80, C81, C82, C83, C84
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O90, C91, C92, C93, C94
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
O80 \\sim C81 \\sim C82 \\sim C83 \\sim C84: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O90 \\sim C91 \\sim C92 \\sim C93 \\sim C94: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
4. Others
 Sof(O90)=Sof(C91)=Sof(H91A)=Sof(H91B)=Sof(C92)=Sof(H92A)=Sof(H92B)=Sof(C93)=
 Sof(H93A)=Sof(H93B)=Sof(C94)=Sof(H94A)=Sof(H94B)=1-FVAR(1)
 Sof(O80)=Sof(C84)=Sof(H84A)=Sof(H84B)=Sof(C83)=Sof(H83A)=Sof(H83B)=Sof(C82)=
 Sof(H82A)=Sof(H82B)=Sof(C81)=Sof(H81A)=Sof(H81B)=FVAR(1)
5.a Free rotating group:
 O80(C84,C83,C82,C81), O90(C91,C92,C93,C94)
5.b Secondary CH2 refined with riding coordinates:
 C84(H84A,H84B), C83(H83A,H83B), C82(H82A,H82B), C81(H81A,H81B), C91(H91A,
 H91B), C92(H92A,H92B), C93(H93A,H93B), C94(H94A,H94B)
5.c Aromatic/amide H refined with riding coordinates:
 N3(H3), C12(H12), C27(H27), C26(H26), C23(H23), C25(H25), C24(H24)
5.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              88819
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'