#------------------------------------------------------------------------------
#$Date: 2021-04-16 11:46:56 +0300 (Fri, 16 Apr 2021) $
#$Revision: 264242 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/33/31/4333131.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4333131
loop_
_publ_author_name
'Panigati, Monica'
'Donghi, Daniela'
'D'Alfonso, Giuseppe'
'Mercandelli, Pierluigi'
'Sironi, Angelo'
'D'Alfonso, Laura'
_publ_section_title
;
 Luminescent Hydrido-Carbonyl Clusters of Rhenium Containing Bridging
 1,2-Diazine Ligands
;
_journal_issue                   26
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10909
_journal_page_last               10921
_journal_paper_doi               10.1021/ic061467z
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C14 H8 N2 O6 Re2'
_chemical_formula_sum            'C14 H8 N2 O6 Re2'
_chemical_formula_weight         672.62
_chemical_name_systematic
;
hexacarbonyldi-μ-hydro(μ-phthalazine-\kN2:\kN3)dirhenium
;
_space_group_IT_number           64
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      64
_symmetry_space_group_name_Hall  '-C 2ac 2'
_symmetry_space_group_name_H-M   'C m c e'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.577(3)
_cell_length_b                   16.197(3)
_cell_length_c                   12.805(3)
_cell_measurement_reflns_used    6380
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      30.5
_cell_measurement_theta_min      2.4
_cell_volume                     3230.7(11)
_computing_structure_refinement
;
Sheldrick, G. M. (1997). SHELX97. Universität Göttingen, Germany.
;
_computing_structure_solution
;
SIR97: Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L.,
Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. &
Spagna, R. (1999). J. Appl. Cryst. 32, 115-119.
;
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
More than a hemisphere of reciprocal space was scanned by 0.3° ω steps,
collecting 1650 frames each at 40 s exposure keeping the detector at 3.0 cm
from the sample. Intensity decay was monitored by recollecting the initial 50
frames at the end of data collection and analysing the duplicate reflections.
;
_diffrn_measurement_device_type  'Brucker SMART'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0515
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20866
_diffrn_reflns_theta_full        30.5
_diffrn_reflns_theta_max         30.5
_diffrn_reflns_theta_min         2.4
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    15.006
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7533
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
Sheldrick, G. M. (1996). SADABS. Universität Göttingen, Germany.
Reflections employed for parameter determination: 9049
Maximum odd and even orders for spherical harmonics: 1 and 4
Effective data to parameter ratio: 9.2
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.766
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2432
_exptl_crystal_preparation
;
A sample of [Re₄(μ₃-H)₄(CO)₁₂] dissolved in dichloromethane
was treated at room temperature with 2 equivalents of phthalazine.
The mixture was left at room temperature overnight. Crystals were isolated
by filtration.
;
_refine_diff_density_max         1.611
_refine_diff_density_min         -1.067
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         2561
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0236
_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)+(0.025P)²] where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0457
_refine_ls_wR_factor_ref         0.0497
_reflns_number_gt                1778
_reflns_number_total             2561
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic061467zsup1.cif
_cod_data_source_block           dimerPHAL(3b)
_cod_depositor_comments
;

2021-04-14
Space group name changed to comply with IUCR recomendations
                 miguel
;
_cod_original_sg_symbol_H-M   'C m c a'
_cod_database_code               4333131
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'x, -y-1/2, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z-1/2'
'x+1/2, -y, z-1/2'
'-x+1/2, y+1/2, 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
Re1 Re 0.410248(9) 0.150355(9) -0.152261(12) 0.03048(6) Uani 1 1 d .
H1 H 0.5000 0.2244 -0.1677 0.043(13) Uiso 1 2 d S
H2 H 0.5000 0.0785 -0.1797 0.043(13) Uiso 1 2 d S
C11 C 0.3220(3) 0.0681(3) -0.1365(3) 0.0401(11) Uani 1 1 d .
C12 C 0.3252(3) 0.2345(3) -0.1264(3) 0.0393(11) Uani 1 1 d .
C13 C 0.3909(3) 0.1574(3) -0.2998(4) 0.0487(12) Uani 1 1 d .
O11 O 0.2701(2) 0.0189(2) -0.1264(3) 0.0581(10) Uani 1 1 d .
O12 O 0.2754(2) 0.2852(2) -0.1129(3) 0.0601(10) Uani 1 1 d .
O13 O 0.3834(3) 0.1608(3) -0.3902(3) 0.0742(12) Uani 1 1 d .
N1 N 0.45534(19) 0.13809(18) 0.0074(2) 0.0289(7) Uani 1 1 d .
C1 C 0.4135(3) 0.1249(2) 0.0956(4) 0.0358(9) Uani 1 1 d .
H11 H 0.3539 0.1260 0.0944 0.043 Uiso 1 1 calc R
C2 C 0.4550(3) 0.1093(2) 0.1914(3) 0.0336(9) Uani 1 1 d .
C3 C 0.4100(4) 0.0924(3) 0.2842(4) 0.0495(12) Uani 1 1 d .
H31 H 0.3503 0.0928 0.2852 0.059 Uiso 1 1 calc R
C4 C 0.4555(4) 0.0752(3) 0.3728(4) 0.0599(15) Uani 1 1 d .
H41 H 0.4263 0.0632 0.4343 0.072 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Re1 0.02408(8) 0.03123(8) 0.03611(9) 0.00114(7) -0.00329(7) 0.00057(7)
C11 0.031(2) 0.040(3) 0.050(3) 0.004(2) -0.0071(18) 0.0031(18)
C12 0.029(2) 0.043(3) 0.046(3) 0.008(2) -0.0019(17) 0.0009(18)
C13 0.043(3) 0.057(3) 0.046(3) 0.002(2) -0.008(2) 0.003(2)
O11 0.044(2) 0.055(2) 0.076(3) 0.0062(17) -0.0091(18) -0.0163(17)
O12 0.039(2) 0.055(2) 0.086(3) 0.0102(19) 0.0103(18) 0.0173(17)
O13 0.081(3) 0.106(4) 0.0356(19) 0.009(2) -0.009(2) 0.004(2)
N1 0.0217(15) 0.0292(18) 0.0358(17) 0.0007(13) 0.0015(13) 0.0007(13)
C1 0.028(2) 0.0321(19) 0.047(2) -0.0010(17) 0.006(2) 0.0031(17)
C2 0.039(2) 0.029(2) 0.033(2) -0.0041(16) 0.0037(18) 0.0031(18)
C3 0.063(3) 0.044(3) 0.042(2) -0.008(2) 0.015(2) -0.003(3)
C4 0.088(4) 0.054(3) 0.038(3) -0.002(2) 0.015(2) -0.002(3)
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'
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
Re1 Re1 C11 135.56(13) 12_655 .
Re1 Re1 C12 133.34(13) 12_655 .
Re1 Re1 C13 99.03(15) 12_655 .
Re1 Re1 N1 71.13(8) 12_655 .
C11 Re1 C12 88.91(19) . .
C11 Re1 C13 91.9(2) . .
C12 Re1 C13 91.10(19) . .
C11 Re1 N1 93.93(15) . .
C12 Re1 N1 97.18(15) . .
C13 Re1 N1 169.95(17) . .
Re1 C11 O11 179.4(4) . .
Re1 C12 O12 178.6(4) . .
Re1 C13 O13 176.7(4) . .
Re1 N1 N1 108.87(8) . 12_655
Re1 N1 C1 131.3(3) . .
N1 N1 C1 119.5(2) 12_655 .
N1 C1 C2 123.2(4) . .
C1 C2 C2 117.3(2) . 12_655
C1 C2 C3 122.8(4) . .
C2 C2 C3 119.9(3) 12_655 .
C2 C3 C4 118.8(5) . .
C3 C4 C4 121.3(3) . 12_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re1 Re1 2.7961(6) 12_655
Re1 C11 1.924(5) .
Re1 C12 1.929(5) .
Re1 C13 1.916(5) .
Re1 N1 2.171(3) .
C11 O11 1.144(5) .
C12 O12 1.142(5) .
C13 O13 1.165(6) .
N1 N1 1.391(6) 12_655
N1 C1 1.321(5) .
C1 C2 1.408(6) .
C2 C2 1.403(9) 12_655
C2 C3 1.407(6) .
C3 C4 1.368(7) .
C4 C4 1.385(12) 12_655
