#------------------------------------------------------------------------------
#$Date: 2019-11-08 02:40:25 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224825 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/80/7058098.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7058098
loop_
_publ_author_name
'Pizarro, Nancy'
'Saldías, Marianela'
'Guzmán, Nicolás'
'Sandoval-Altamirano, Catalina'
'Kahlal, Samia'
'Saillard, Jean-Yves'
'Hamon, Jean-René'
'Vega, Andrés'
_publ_section_title
;
 1IL and 3MLCT excited states modulated by H+: the structure and
 photophysical properties of
 [(2-bromo-5-(1H-pyrazol-1-yl)pyrazine)Re(CO)3Br]
;
_journal_issue                   6
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2449
_journal_paper_doi               10.1039/C8NJ04196B
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C10 H5 Br2 N4 O3 Re'
_chemical_formula_sum            'C10 H5 Br2 N4 O3 Re'
_chemical_formula_weight         575.20
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-09-20 deposited with the CCDC.
2019-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                106.008(7)
_cell_angle_beta                 102.690(6)
_cell_angle_gamma                91.343(7)
_cell_formula_units_Z            2
_cell_length_a                   6.769(4)
_cell_length_b                   8.079(4)
_cell_length_c                   13.343(7)
_cell_measurement_reflns_used    4070
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.94
_cell_measurement_theta_min      2.64
_cell_volume                     681.5(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0655
_diffrn_reflns_av_unetI/netI     0.0853
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5316
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         1.634
_exptl_absorpt_coefficient_mu    14.788
_exptl_absorpt_correction_T_max  0.2565
_exptl_absorpt_correction_T_min  0.0324
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS, Bruker'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.803
_exptl_crystal_description       stick
_exptl_crystal_F_000             524
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Chloroform'
_exptl_crystal_size_max          0.194
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.057
_refine_diff_density_max         3.549
_refine_diff_density_min         -1.962
_refine_diff_density_rms         0.277
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2664
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0517
_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/[σ²(Fo²)+(0.0565P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1233
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2181
_reflns_number_total             2664
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8nj04196b2.cif
_cod_data_source_block           SCD17_37_P1
_cod_depositor_comments
'Adding full bibliography for 7058098--7058099.cif.'
_cod_original_cell_volume        681.6(6)
_cod_database_code               7058098
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.185
_shelx_estimated_absorpt_t_max   0.430
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Re1 Re 0.04886(6) 0.22828(6) 0.32444(3) 0.03393(18) Uani 1 1 d . .
Br1 Br 0.15453(19) 0.25574(17) 0.15226(9) 0.0483(3) Uani 1 1 d . .
N1 N 0.2675(14) 0.0363(12) 0.3250(7) 0.036(2) Uani 1 1 d . .
N2 N 0.1909(14) -0.1276(13) 0.2647(7) 0.036(2) Uani 1 1 d . .
N3 N -0.1149(14) -0.0177(13) 0.2184(7) 0.039(2) Uani 1 1 d . .
N4 N -0.2847(19) -0.3329(15) 0.0785(9) 0.060(3) Uani 1 1 d . .
C1 C 0.4575(18) 0.0269(17) 0.3743(8) 0.043(3) Uani 1 1 d . .
H1 H 0.5462 0.1195 0.4208 0.051 Uiso 1 1 calc R U
C2 C 0.5041(19) -0.1507(19) 0.3440(10) 0.052(3) Uani 1 1 d . .
H2 H 0.6265 -0.1939 0.3672 0.063 Uiso 1 1 calc R U
C3 C 0.3369(19) -0.2409(17) 0.2760(9) 0.043(3) Uani 1 1 d . .
H3 H 0.3218 -0.3593 0.2423 0.052 Uiso 1 1 calc R U
C4 C -0.0115(17) -0.1597(16) 0.2045(8) 0.039(3) Uani 1 1 d . .
C5 C -0.098(2) -0.3156(17) 0.1341(10) 0.051(3) Uani 1 1 d . .
H5 H -0.0211 -0.4105 0.1260 0.062 Uiso 1 1 calc R U
C6 C -0.3872(18) -0.1966(16) 0.0905(9) 0.045(3) Uani 1 1 d . .
C7 C -0.3078(16) -0.0335(15) 0.1624(8) 0.039(3) Uani 1 1 d . .
H7 H -0.3867 0.0598 0.1707 0.047 Uiso 1 1 calc R U
Br2 Br -0.66124(19) -0.21743(18) 0.01042(9) 0.0512(3) Uani 1 1 d . .
C13 C -0.167(2) 0.3760(15) 0.3086(9) 0.043(3) Uani 1 1 d . .
O13 O -0.2933(15) 0.4670(13) 0.2991(7) 0.065(3) Uani 1 1 d . .
C14 C 0.2238(19) 0.4284(19) 0.4077(9) 0.047(3) Uani 1 1 d . .
O14 O 0.3260(14) 0.5563(13) 0.4547(8) 0.063(3) Uani 1 1 d . .
C15 C -0.0118(15) 0.2007(14) 0.4562(9) 0.035(2) Uani 1 1 d . .
O15 O -0.0347(15) 0.1889(13) 0.5324(8) 0.061(3) Uani 1 1 d . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 1.00 -1.00 0.0370
0.00 -1.00 1.00 0.0230
-2.00 0.00 1.00 0.0950
2.00 0.00 -1.00 0.0420
0.00 -2.00 -1.00 0.0280
0.00 2.00 1.00 0.0140
-2.00 -1.00 -2.00 0.0820
2.00 1.00 2.00 0.0380
0.00 0.00 -1.00 0.0480
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
C14 Re1 C13 88.0(5) y
C14 Re1 C15 89.2(5) y
C13 Re1 C15 91.2(4) y
C14 Re1 N1 99.1(4) y
C13 Re1 N1 172.6(4) y
C15 Re1 N1 91.0(4) y
C14 Re1 N3 171.5(4) y
C13 Re1 N3 98.8(4) y
C15 Re1 N3 95.8(4) y
N1 Re1 N3 73.9(3) y
C14 Re1 Br1 90.0(3) y
C13 Re1 Br1 92.8(3) y
C15 Re1 Br1 175.9(3) y
N1 Re1 Br1 85.2(2) y
N3 Re1 Br1 84.6(2) y
C1 N1 N2 107.1(10) ?
C1 N1 Re1 138.2(8) ?
N2 N1 Re1 114.5(6) ?
N1 N2 C3 110.0(10) ?
N1 N2 C4 120.4(9) ?
C3 N2 C4 129.7(11) ?
C7 N3 C4 117.8(10) ?
C7 N3 Re1 124.1(8) ?
C4 N3 Re1 118.0(7) ?
C5 N4 C6 118.0(12) ?
N1 C1 C2 108.7(11) ?
N1 C1 H1 125.6 ?
C2 C1 H1 125.6 ?
C3 C2 C1 106.5(11) ?
C3 C2 H2 126.8 ?
C1 C2 H2 126.8 ?
C2 C3 N2 107.8(12) ?
C2 C3 H3 126.1 ?
N2 C3 H3 126.1 ?
N3 C4 C5 121.8(11) ?
N3 C4 N2 113.1(10) ?
C5 C4 N2 125.0(11) ?
N4 C5 C4 121.0(12) ?
N4 C5 H5 119.5 ?
C4 C5 H5 119.5 ?
N4 C6 C7 123.5(11) ?
N4 C6 Br2 119.1(9) ?
C7 C6 Br2 117.4(9) ?
N3 C7 C6 117.7(11) ?
N3 C7 H7 121.1 ?
C6 C7 H7 121.1 ?
O13 C13 Re1 178.7(11) ?
O14 C14 Re1 176.1(11) ?
O15 C15 Re1 176.0(10) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Re1 C14 1.895(15) y
Re1 C13 1.918(14) y
Re1 C15 1.959(12) y
Re1 N1 2.169(9) y
Re1 N3 2.199(10) y
Re1 Br1 2.6144(16) y
N1 C1 1.324(14) ?
N1 N2 1.366(13) ?
N2 C3 1.375(14) ?
N2 C4 1.405(14) ?
N3 C7 1.338(13) ?
N3 C4 1.349(14) ?
N4 C5 1.303(17) ?
N4 C6 1.306(16) ?
C1 C2 1.442(18) ?
C1 H1 0.9300 ?
C2 C3 1.334(18) ?
C2 H2 0.9300 ?
C3 H3 0.9300 ?
C4 C5 1.371(18) ?
C5 H5 0.9300 ?
C6 C7 1.410(16) ?
C6 Br2 1.904(12) ?
C7 H7 0.9300 ?
C13 O13 1.152(14) ?
C14 O14 1.165(16) ?
C15 O15 1.091(13) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C5 H5 Br1 0.93 3.05 3.940(13) 161.0 1_545
C3 H3 Br1 0.93 3.09 3.994(14) 163.2 1_545
