#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:59:17 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179434 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/31/4333133.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_4333133
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         'C28 H16 N4 O12 Re4, C H2 Cl2'
_chemical_formula_sum            'C29 H18 Cl2 N4 O12 Re4'
_chemical_formula_weight         1430.18
_chemical_name_systematic
;
dodecacarbonyltetra-μ-hydrobis(μ-phthalazine-\kN2:\kN3)tetrarhenium
dichloromethane solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 98.84(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.858(3)
_cell_length_b                   9.760(3)
_cell_length_c                   17.527(5)
_cell_measurement_reflns_used    4991
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      30.6
_cell_measurement_theta_min      2.1
_cell_volume                     1835.3(9)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  'Siemens SMART'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0657
_diffrn_reflns_av_sigmaI/netI    0.0615
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            24265
_diffrn_reflns_theta_full        30.6
_diffrn_reflns_theta_max         30.6
_diffrn_reflns_theta_min         2.1
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    13.356
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5692
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
Sheldrick, G. M. (1996). SADABS. Universität Göttingen, Germany.
Reflections employed for parameter determination: 13690
Maximum odd and even orders for spherical harmonics: 1 and 4
Effective data to parameter ratio: 12.0
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.588
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1300
_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         1.624
_refine_diff_density_min         -1.204
_refine_diff_density_rms         0.263
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.889
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         5601
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0335
_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)+(0.038P)²] where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0750
_reflns_number_gt                4014
_reflns_number_total             5601
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic061467zsup1.cif
_cod_data_source_block           squarePHAL(4b)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4333133
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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_group
Re1 Re 0.12020(2) 0.13178(3) 0.093868(13) 0.02302(7) Uani 1 1 d . 1
Re2 Re -0.12670(2) 0.19744(2) -0.027792(14) 0.02228(7) Uani 1 1 d . 1
H1 H -0.0504 0.1576 0.0715 0.054(17) Uiso 1 1 d . 1
H2 H 0.0681 -0.0242 0.0404 0.054(17) Uiso 1 1 d . 1
C11 C 0.1299(7) 0.3191(7) 0.1340(4) 0.0345(16) Uani 1 1 d . 1
C12 C 0.2923(8) 0.1027(8) 0.1351(4) 0.0386(17) Uani 1 1 d . 1
C13 C 0.0758(7) 0.0542(7) 0.1875(4) 0.0359(16) Uani 1 1 d . 1
C21 C -0.1403(7) 0.3838(8) 0.0076(5) 0.0383(17) Uani 1 1 d . 1
C22 C -0.2280(7) 0.2367(7) -0.1267(4) 0.0344(15) Uani 1 1 d . 1
C23 C -0.2762(7) 0.1520(7) 0.0097(4) 0.0346(16) Uani 1 1 d . 1
O11 O 0.1301(6) 0.4270(6) 0.1573(3) 0.0587(17) Uani 1 1 d . 1
O12 O 0.3926(6) 0.0866(7) 0.1633(4) 0.0657(19) Uani 1 1 d . 1
O13 O 0.0503(7) 0.0028(7) 0.2409(3) 0.0624(18) Uani 1 1 d . 1
O21 O -0.1471(6) 0.4938(6) 0.0306(4) 0.0606(17) Uani 1 1 d . 1
O22 O -0.2856(6) 0.2563(7) -0.1850(3) 0.0619(18) Uani 1 1 d . 1
O23 O -0.3683(5) 0.1234(7) 0.0322(4) 0.0585(17) Uani 1 1 d . 1
N1 N 0.1538(5) 0.1905(5) -0.0213(3) 0.0217(10) Uani 1 1 d . 1
N2 N 0.0491(5) 0.2274(5) -0.0729(3) 0.0243(11) Uani 1 1 d . 1
C1 C 0.0614(6) 0.2597(7) -0.1434(4) 0.0309(14) Uani 1 1 d . 1
H11 H -0.0087 0.2916 -0.1757 0.037 Uiso 1 1 calc R 1
C2 C 0.1742(7) 0.2493(8) -0.1743(4) 0.0339(15) Uani 1 1 d . 1
C3 C 0.1820(9) 0.2731(12) -0.2533(5) 0.060(3) Uani 1 1 d . 1
H31 H 0.1133 0.3031 -0.2875 0.072 Uiso 1 1 calc R 1
C4 C 0.2949(9) 0.2501(14) -0.2774(5) 0.075(3) Uani 1 1 d . 1
H41 H 0.3024 0.2668 -0.3287 0.090 Uiso 1 1 calc R 1
C5 C 0.3976(8) 0.2029(12) -0.2277(5) 0.063(3) Uani 1 1 d . 1
H51 H 0.4718 0.1861 -0.2465 0.076 Uiso 1 1 calc R 1
C6 C 0.3912(8) 0.1808(10) -0.1510(5) 0.051(2) Uani 1 1 d . 1
H61 H 0.4605 0.1493 -0.1177 0.061 Uiso 1 1 calc R 1
C7 C 0.2792(7) 0.2062(8) -0.1237(4) 0.0337(15) Uani 1 1 d . 1
C8 C 0.2622(7) 0.1819(7) -0.0469(4) 0.0312(14) Uani 1 1 d . 1
H81 H 0.3319 0.1581 -0.0116 0.037 Uiso 1 1 calc R 1
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
Re2 Re1 Re2 91.210(13) . 3
Re2 Re1 C11 92.6(2) . .
Re2 Re1 C12 160.4(2) . .
Re2 Re1 C13 110.4(2) . .
Re2 Re1 N1 64.92(13) . .
Re2 Re1 C11 175.7(2) 3 .
Re2 Re1 C12 85.4(2) 3 .
Re2 Re1 C13 86.6(2) 3 .
Re2 Re1 N1 85.32(13) 3 .
C11 Re1 C12 90.4(3) . .
C11 Re1 C13 93.9(3) . .
C11 Re1 N1 94.6(2) . .
C12 Re1 C13 88.7(3) . .
C12 Re1 N1 95.5(3) . .
C13 Re1 N1 170.5(2) . .
Re1 Re2 Re1 88.790(13) . 3
Re1 Re2 C21 94.1(2) . .
Re1 Re2 C22 158.2(2) . .
Re1 Re2 C23 113.2(2) . .
Re1 Re2 N2 65.40(13) . .
Re1 Re2 C21 176.8(2) 3 .
Re1 Re2 C22 85.5(2) 3 .
Re1 Re2 C23 87.8(2) 3 .
Re1 Re2 N2 86.50(13) 3 .
C21 Re2 C22 92.3(3) . .
C21 Re2 C23 89.9(3) . .
C21 Re2 N2 95.9(3) . .
C22 Re2 C23 87.6(3) . .
C22 Re2 N2 93.3(3) . .
C23 Re2 N2 174.1(2) . .
Re1 C11 O11 177.1(7) . .
Re1 C12 O12 176.3(7) . .
Re1 C13 O13 176.8(7) . .
Re2 C21 O21 178.1(8) . .
Re2 C22 O22 178.1(7) . .
Re2 C23 O23 179.5(7) . .
Re1 N1 N2 115.7(4) . .
Re1 N1 C8 125.4(4) . .
N2 N1 C8 118.6(5) . .
Re2 N2 N1 113.7(4) . .
Re2 N2 C1 126.5(5) . .
N1 N2 C1 119.2(6) . .
N2 C1 C2 124.5(6) . .
C1 C2 C3 123.1(7) . .
C1 C2 C7 116.5(6) . .
C3 C2 C7 120.3(7) . .
C2 C3 C4 117.5(8) . .
C3 C4 C5 122.1(8) . .
C4 C5 C6 120.7(8) . .
C5 C6 C7 119.0(8) . .
C2 C7 C6 120.3(7) . .
C2 C7 C8 116.5(6) . .
C6 C7 C8 123.2(7) . .
N1 C8 C7 124.5(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re1 Re2 3.2232(8) .
Re1 Re2 3.4199(10) 3
Re1 C11 1.956(6) .
Re1 C12 1.918(8) .
Re1 C13 1.935(7) .
Re1 N1 2.183(5) .
Re2 C21 1.935(8) .
Re2 C22 1.943(7) .
Re2 C23 1.895(8) .
Re2 N2 2.195(5) .
C11 O11 1.129(8) .
C12 O12 1.136(9) .
C13 O13 1.133(8) .
C21 O21 1.153(9) .
C22 O22 1.129(8) .
C23 O23 1.164(9) .
N1 N2 1.387(7) .
N1 C8 1.325(8) .
N2 C1 1.303(8) .
C1 C2 1.418(9) .
C2 C3 1.418(10) .
C2 C7 1.398(10) .
C3 C4 1.374(12) .
C4 C5 1.384(13) .
C5 C6 1.374(12) .
C6 C7 1.396(10) .
C7 C8 1.406(9) .
