#------------------------------------------------------------------------------
#$Date: 2018-02-01 14:52:20 +0200 (Thu, 01 Feb 2018) $
#$Revision: 206022 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/00/95/2009549.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# 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_2009549
loop_
_publ_author_name
'Mayo, S.C.'
'Brown, M.'
'Lloyd, V.K.'
_publ_section_title
;
 A zirconium polyhydride dimer, [Zr₂H₄(BH₄)₄(PMe₃)₄]
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              367
_journal_page_last               369
_journal_paper_doi               10.1107/S0108270193008042
_journal_volume                  50
_journal_year                    1994
_chemical_formula_sum            'C12 H56 B4 P4 Zr2'
_chemical_formula_weight         550.16
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n :2'
_atom_type_scat_source
' CRYSTALS (Watkin, Carruthers & Betteridge, 1985)'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.516(7)
_cell_length_b                   13.516(7)
_cell_length_c                   10.353(5)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    296
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10.5
_cell_volume                     1891.3(17)
_diffrn_measurement_device       'Stoe Stadi-4'
_diffrn_measurement_method       'learnt profile'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2076
_diffrn_reflns_theta_max         25
_diffrn_standards_decay_%        -15
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.707
_exptl_absorpt_correction_T_max  0.6157
_exptl_absorpt_correction_T_min  0.5334
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'deep green'
_exptl_crystal_density_diffrn    0.967
_exptl_crystal_description       cuboid
_exptl_crystal_size_max          0.456
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.380
_refine_diff_density_max         0.41
_refine_diff_density_min         -0.45
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.82
_refine_ls_number_parameters     65
_refine_ls_number_reflns         874
_refine_ls_R_factor_obs          0.062
_refine_ls_shift/esd_max         0.1
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme
' Weights based on 3rd order Chebychev polynomial in F~c~'
_refine_ls_wR_factor_obs         0.054
_reflns_number_observed          874
_reflns_number_total             1674
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            mu1053.cif
_cod_data_source_block           mu1053_structure_1_of_1
_cod_original_cell_volume        1891.3
_cod_database_code               2009549
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -y+1/2,x,z
3 -x+1/2,-y+1/2,z
4 y,-x+1/2,z
5 -x,-y,-z
6 y+1/2,-x,-z
7 x+1/2,y+1/2,-z
8 -y,x+1/2,-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
Zr .7500 .2500 .14389(7) .0559
P .8791(2) .3992(2) .2049(2) .0790
C(1) .9030(10) .4170(10) .3740(10) .1045
C(2) .8434(9) .5227(8) .1490(10) .1172
C(3) 1.0011(9) .3810(10) .1340(10) .1174
B .6307(9) .3608(8) .2750(10) .0805
H(11) .885(5) .477(4) .455(4) ?
H(12) .968(3) .377(4) .397(5) ?
H(13) .857(4) .362(4) .431(4) ?
H(21) .890(4) .584(3) .171(6) ?
H(22) .844(5) .509(4) .0400(10) ?
H(23) .762(2) .544(4) .170(6) ?
H(31) 1.058(3) .433(4) .162(6) ?
H(32) 1.018(3) .317(2) .167(6) ?
H(33) .987(3) .389(5) .043(2) ?
H(100) .7410 .3580 .0010 ?
H(101) .5490(10) .338(3) .269(6) ?
H(102) .653(4) .374(4) .178(2) ?
H(103) .639(4) .438(2) .328(5) ?
H(104) .678(3) .303(2) .322(4) ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
P Zr P . 18_555 153.40(10) yes
B Zr B . 18_555 116.7(6) yes
Zr Zr P 17_555 . 103.32(5) yes
Zr Zr B 17_555 . 121.6(3) yes
Zr H(100) Zr . 17_555 91 yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Zr Zr . 17_555 2.9790(10) yes
Zr P . . 2.740(3) yes
Zr B . . 2.590(10) yes
P C(1) . . 1.800(10) yes
P C(3) . . 1.820(10) yes
Zr H(100) . . 2.08 yes
Zr H(100) 17_555 . 2.10 yes
Zr H(102) . . 2.16(5) yes
Zr H(104) . . 2.20(5) yes
P C(2) . . 1.830(10) yes
C(1) H(11) . . 1.188 no
C(1) H(12) . . 1.062 no
C(1) H(13) . . 1.125 no
C(2) H(21) . . 1.063 no
C(2) H(22) . . 1.146 no
C(2) H(23) . . 1.158 no
C(3) H(31) . . 1.083 no
C(3) H(32) . . .963 no
C(3) H(33) . . .969 no
B H(101) . . 1.144 no
B H(102) . . 1.063 no
B H(103) . . 1.183 no
B H(104) . . 1.126 no
