#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:28:34 +0100 (vie 25 de mar de 2016) $
#$Revision: 179846 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/42/7014297.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_7014297
loop_
_publ_author_name
'Isabel Santos'
'Susana Alves'
'Joao D. G. Correia'
'Angela Domingos'
'Antonio Paulo'
_publ_section_title
;
 Coordination capabilities of pyrazolyl containing ligands towards the
 fac-[Re(CO)3]+ moiety
;
_journal_issue                   24
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              4714
_journal_page_last               4719
_journal_paper_doi               10.1039/b207164a
_journal_year                    2002
_chemical_formula_moiety         '[Re(CO)3(k3-pz(CH2)2NH(CH2)2NH2)]Br'
_chemical_formula_sum            'C12 H18 Br N4 O3 Re'
_chemical_formula_weight         532.41
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.582(18)
_cell_angle_beta                 85.696(13)
_cell_angle_gamma                74.688(14)
_cell_formula_units_Z            2
_cell_length_a                   8.6270(11)
_cell_length_b                   9.0940(15)
_cell_length_c                   10.7625(16)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.8
_cell_measurement_theta_min      7.5
_cell_volume                     812.1(2)
_computing_cell_refinement       'CAD4 software(Enraf-Nonius,1989)'
_computing_data_collection       'CAD4 software(Enraf-Nonius,1989)'
_computing_data_reduction        process-MolEN(Fair,1990)
_computing_molecular_graphics    'ORTEP-3 (Farrugia,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97(Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  CAD4-Enraf-Nonius
_diffrn_measurement_method       ω/2\qscans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0140
_diffrn_reflns_av_sigmaI/netI    0.0231
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3747
_diffrn_reflns_theta_full        27.04
_diffrn_reflns_theta_max         27.04
_diffrn_reflns_theta_min         1.90
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    9.956
_exptl_absorpt_correction_T_max  0.9948
_exptl_absorpt_correction_T_min  0.5474
_exptl_absorpt_correction_type   'empirical via \y-scan North et al(1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.177
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.27
_refine_diff_density_max         1.621
_refine_diff_density_min         -1.169
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3507
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0426P)²+2.6865P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0734
_reflns_number_gt                3179
_reflns_number_total             3507
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b207164a.txt
_cod_data_source_block           pznhnh2
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7014297
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.69016(3) 0.80249(2) 0.79640(2) 0.03017(8) Uani 1 1 d . . .
Br1 Br 0.24559(8) 0.82853(8) 0.54461(7) 0.04825(16) Uani 1 1 d . . .
O1 O 0.8059(7) 0.9610(6) 1.0052(5) 0.0612(14) Uani 1 1 d . . .
O2 O 0.4450(7) 1.1088(6) 0.7594(5) 0.0691(16) Uani 1 1 d . . .
O3 O 0.4578(7) 0.7230(7) 0.9987(5) 0.0699(16) Uani 1 1 d . . .
N1 N 0.8528(6) 0.8440(6) 0.6389(4) 0.0368(11) Uani 1 1 d . . .
H1A H 0.8241 0.9433 0.6175 0.044 Uiso 1 1 calc R . .
H1B H 0.9544 0.8214 0.6624 0.044 Uiso 1 1 calc R . .
N2 N 0.6103(6) 0.6951(6) 0.6377(5) 0.0427(12) Uani 1 1 d . . .
H2 H 0.5020 0.7367 0.6393 0.051 Uiso 1 1 calc R . .
N3 N 0.8715(6) 0.5827(5) 0.8094(5) 0.0348(10) Uani 1 1 d . . .
N31 N 0.8345(6) 0.4488(5) 0.7871(4) 0.0353(10) Uani 1 1 d . . .
C1 C 0.7682(8) 0.8981(7) 0.9254(6) 0.0394(13) Uani 1 1 d . . .
C2 C 0.5343(8) 0.9932(7) 0.7729(6) 0.0431(14) Uani 1 1 d . . .
C3 C 0.5464(8) 0.7529(8) 0.9220(6) 0.0452(15) Uani 1 1 d . . .
C4 C 0.6730(8) 0.4489(7) 0.7577(7) 0.0502(17) Uani 1 1 d . . .
H4A H 0.5962 0.4991 0.8239 0.060 Uiso 1 1 calc R . .
H4B H 0.6657 0.3446 0.7525 0.060 Uiso 1 1 calc R . .
C5 C 0.6306(10) 0.5305(8) 0.6352(8) 0.063(2) Uani 1 1 d . . .
H5A H 0.7149 0.4867 0.5716 0.076 Uiso 1 1 calc R . .
H5B H 0.5315 0.5116 0.6111 0.076 Uiso 1 1 calc R . .
C6 C 0.6769(9) 0.7543(10) 0.5194(7) 0.0569(18) Uani 1 1 d . . .
H6A H 0.6687 0.6918 0.4497 0.068 Uiso 1 1 calc R . .
H6B H 0.6151 0.8580 0.5038 0.068 Uiso 1 1 calc R . .
C7 C 0.8463(10) 0.7509(10) 0.5309(7) 0.0588(19) Uani 1 1 d . . .
H7A H 0.9098 0.6469 0.5426 0.071 Uiso 1 1 calc R . .
H7B H 0.8896 0.7917 0.4559 0.071 Uiso 1 1 calc R . .
C31 C 0.9648(9) 0.3295(7) 0.7933(6) 0.0425(14) Uani 1 1 d . . .
C32 C 1.0895(8) 0.3876(8) 0.8202(6) 0.0454(15) Uani 1 1 d . . .
H32 H 1.1952 0.3323 0.8297 0.055 Uiso 1 1 calc R . .
C33 C 1.0285(7) 0.5450(7) 0.8306(5) 0.0363(12) Uani 1 1 d . . .
C34 C 1.1171(8) 0.6560(8) 0.8622(6) 0.0472(15) Uani 1 1 d . . .
H34A H 1.0462 0.7571 0.8617 0.071 Uiso 1 1 calc R . .
H34B H 1.2063 0.6500 0.8019 0.071 Uiso 1 1 calc R . .
H34C H 1.1562 0.6332 0.9435 0.071 Uiso 1 1 calc R . .
C35 C 0.9598(11) 0.1700(8) 0.7749(7) 0.061(2) Uani 1 1 d . . .
H35A H 0.8537 0.1686 0.7547 0.092 Uiso 1 1 calc R . .
H35B H 0.9859 0.1127 0.8501 0.092 Uiso 1 1 calc R . .
H35C H 1.0366 0.1253 0.7081 0.092 Uiso 1 1 calc R . .
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'
Br Br -0.2901 2.4595 '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'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 Re1 C1 86.3(3) . . ?
C3 Re1 C2 88.7(3) . . ?
C1 Re1 C2 87.6(3) . . ?
C3 Re1 N1 174.6(2) . . ?
C1 Re1 N1 98.9(2) . . ?
C2 Re1 N1 93.1(2) . . ?
C3 Re1 N3 94.2(2) . . ?
C1 Re1 N3 95.2(2) . . ?
C2 Re1 N3 176.1(2) . . ?
N1 Re1 N3 83.85(19) . . ?
C3 Re1 N2 97.3(2) . . ?
C1 Re1 N2 176.5(2) . . ?
C2 Re1 N2 92.5(2) . . ?
N1 Re1 N2 77.53(19) . . ?
N3 Re1 N2 84.50(19) . . ?
C7 N1 Re1 111.0(4) . . ?
C5 N2 C6 112.6(6) . . ?
C5 N2 Re1 120.6(4) . . ?
C6 N2 Re1 107.5(4) . . ?
C33 N3 N31 106.1(5) . . ?
C33 N3 Re1 132.9(4) . . ?
N31 N3 Re1 120.8(3) . . ?
C31 N31 N3 111.0(5) . . ?
C31 N31 C4 128.5(5) . . ?
N3 N31 C4 120.6(5) . . ?
O1 C1 Re1 175.8(6) . . ?
O2 C2 Re1 178.0(7) . . ?
O3 C3 Re1 179.7(7) . . ?
N31 C4 C5 111.1(6) . . ?
N2 C5 C4 114.7(6) . . ?
C7 C6 N2 109.5(6) . . ?
N1 C7 C6 107.7(6) . . ?
N31 C31 C32 106.6(5) . . ?
N31 C31 C35 122.8(6) . . ?
C32 C31 C35 130.5(6) . . ?
C33 C32 C31 107.2(5) . . ?
N3 C33 C32 109.0(5) . . ?
N3 C33 C34 124.0(6) . . ?
C32 C33 C34 127.0(6) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 C3 1.893(7) . ?
Re1 C1 1.909(6) . ?
Re1 C2 1.918(6) . ?
Re1 N1 2.208(5) . ?
Re1 N3 2.198(5) . ?
Re1 N2 2.227(5) . ?
O1 C1 1.156(8) . ?
O2 C2 1.141(8) . ?
O3 C3 1.159(8) . ?
N1 C7 1.468(8) . ?
N2 C5 1.461(9) . ?
N2 C6 1.504(9) . ?
N3 C33 1.342(7) . ?
N3 N31 1.369(6) . ?
N31 C31 1.345(8) . ?
N31 C4 1.451(8) . ?
C4 C5 1.518(11) . ?
C6 C7 1.468(10) . ?
C31 C32 1.369(10) . ?
C31 C35 1.481(9) . ?
C32 C33 1.392(9) . ?
C33 C34 1.477(9) . ?
