#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:01:19 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180368 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/37/7203734.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_7203734
loop_
_publ_author_name
'McMurtrie, John'
'Dance, Ian'
_publ_section_title
;
 Engineering the metal-terpy grid with complexes containing 4?-hydroxy
 terpyridine
;
_journal_issue                   36
_journal_name_full               CrystEngComm
_journal_page_first              230
_journal_paper_doi               10.1039/b500989h
_journal_volume                  7
_journal_year                    2005
_chemical_formula_sum            'C30 H22 B2 F8 N6 O2 Ru'
_chemical_formula_weight         773.25
_chemical_name_systematic
;
[Ru(terpy)(terpyOH)](BF4)2.H2O
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 99.557(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            2
_cell_length_a                   8.7533(10)
_cell_length_b                   8.9226(10)
_cell_length_c                   19.8607(23)
_cell_measurement_reflns_used    984
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.220
_cell_measurement_theta_min      3.086
_cell_volume                     1529.6(3)
_computing_cell_refinement       'SAINT (Bruker,1995)'
_computing_data_collection       'SMART (Bruker,1995)'
_computing_data_reduction        'SAINT and XPREP (Bruker 1995)'
_computing_molecular_graphics    'teXsan for Windows (MSC, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, et. al. 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_sigmaI/netI    0.0173
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            13657
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.04
_diffrn_standards_decay_%        0.01
_diffrn_standards_number         298
_exptl_absorpt_coefficient_mu    0.602
_exptl_absorpt_correction_T_max  0.94901
_exptl_absorpt_correction_T_min  0.78725
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'Gaussian (XPREP,Bruker 1995; Coppens,1965)'
_exptl_crystal_colour            'intense red'
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.243
_refine_diff_density_min         -0.960
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         6943
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0648P)²+2.7438P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1099
_reflns_number_gt                6838
_reflns_number_total             6943
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b500989h.txt
_cod_data_source_block           crystal_3b
_cod_original_cell_volume        1529.7(13)
_cod_original_sg_symbol_H-M      P21
_cod_database_code               7203734
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.73834(3) 0.26487(4) 0.241414(12) 0.01898(8) Uani 1 1 d . . .
N1 N 0.8350(4) 0.0566(4) 0.27192(17) 0.0224(6) Uani 1 1 d . . .
N2 N 0.7478(3) 0.2763(7) 0.34203(14) 0.0197(6) Uani 1 1 d . . .
N3 N 0.6531(3) 0.4796(4) 0.25229(17) 0.0195(6) Uani 1 1 d . . .
N4 N 0.9511(4) 0.3537(4) 0.22967(19) 0.0231(7) Uani 1 1 d . . .
N5 N 0.7269(4) 0.2476(5) 0.14124(15) 0.0210(8) Uani 1 1 d . . .
N6 N 0.5184(4) 0.1749(4) 0.21262(17) 0.0210(6) Uani 1 1 d . . .
B1 B 0.2519(8) 0.3208(10) 0.4459(3) 0.067(2) Uani 1 1 d D . .
F1 F 0.1110(4) 0.3731(5) 0.4436(2) 0.0611(9) Uiso 1 1 d D . .
F2 F 0.3283(5) 0.2931(6) 0.5099(2) 0.0819(13) Uiso 1 1 d D . .
F3 F 0.2890(7) 0.2361(8) 0.3970(3) 0.1120(18) Uiso 1 1 d D . .
F4 F 0.3339(9) 0.4583(8) 0.4308(4) 0.135(2) Uiso 1 1 d D . .
B2 B 0.8107(7) -0.2312(9) 0.0579(2) 0.0447(11) Uani 1 1 d D . .
F5 F 0.7045(5) -0.1688(5) 0.09383(17) 0.0629(10) Uani 1 1 d D . .
F6 F 0.7814(5) -0.3825(4) 0.0538(2) 0.0718(12) Uani 1 1 d D . .
F7 F 0.9626(4) -0.2056(6) 0.09128(18) 0.0718(14) Uani 1 1 d D . .
F8 F 0.7901(5) -0.1715(5) -0.00665(19) 0.0659(11) Uani 1 1 d D . .
C1 C 0.8795(4) -0.0505(5) 0.2322(2) 0.0253(8) Uani 1 1 d . . .
H1 H 0.8636 -0.0353 0.1842 0.030 Uiso 1 1 calc R . .
C2 C 0.9484(5) -0.1835(5) 0.2586(3) 0.0322(9) Uani 1 1 d . . .
H2 H 0.9782 -0.2580 0.2292 0.039 Uiso 1 1 calc R . .
C3 C 0.9726(5) -0.2052(5) 0.3288(3) 0.0341(11) Uani 1 1 d . . .
H3 H 1.0203 -0.2945 0.3481 0.041 Uiso 1 1 calc R . .
C4 C 0.9262(5) -0.0948(5) 0.3706(2) 0.0304(9) Uani 1 1 d . . .
H4 H 0.9418 -0.1079 0.4187 0.037 Uiso 1 1 calc R . .
C5 C 0.8569(4) 0.0347(4) 0.3412(2) 0.0219(7) Uani 1 1 d . . .
C6 C 0.8039(4) 0.1581(5) 0.3814(2) 0.0220(7) Uani 1 1 d . . .
C7 C 0.8078(5) 0.1606(5) 0.4515(2) 0.0271(8) Uani 1 1 d . . .
H7 H 0.8492 0.0785 0.4791 0.033 Uiso 1 1 calc R . .
C8 C 0.7498(5) 0.2861(6) 0.48055(19) 0.0284(10) Uani 1 1 d . . .
C9 C 0.6937(5) 0.4088(5) 0.4391(2) 0.0275(8) Uani 1 1 d . . .
H9 H 0.6566 0.4963 0.4584 0.033 Uiso 1 1 calc R . .
C10 C 0.6938(4) 0.3983(5) 0.3694(2) 0.0216(7) Uani 1 1 d . . .
C11 C 0.6396(4) 0.5151(4) 0.3183(2) 0.0214(7) Uani 1 1 d . . .
C12 C 0.5809(5) 0.6528(5) 0.3341(2) 0.0269(8) Uani 1 1 d . . .
H12 H 0.5700 0.6749 0.3798 0.032 Uiso 1 1 calc R . .
C13 C 0.5386(4) 0.7571(7) 0.2835(2) 0.0296(7) Uani 1 1 d . . .
H13 H 0.4968 0.8509 0.2939 0.036 Uiso 1 1 calc R . .
C14 C 0.5575(5) 0.7237(4) 0.2175(2) 0.0276(9) Uani 1 1 d . . .
H14 H 0.5317 0.7956 0.1821 0.033 Uiso 1 1 calc R . .
C15 C 0.6148(4) 0.5838(5) 0.2033(2) 0.0232(8) Uani 1 1 d . . .
H15 H 0.6273 0.5611 0.1578 0.028 Uiso 1 1 calc R . .
C16 C 1.0595(5) 0.4097(5) 0.2784(3) 0.0294(9) Uani 1 1 d . . .
H16 H 1.0451 0.4035 0.3246 0.035 Uiso 1 1 calc R . .
C17 C 1.1936(5) 0.4772(6) 0.2631(3) 0.0402(12) Uani 1 1 d . . .
H17 H 1.2692 0.5166 0.2986 0.048 Uiso 1 1 calc R . .
C18 C 1.2155(6) 0.4862(6) 0.1958(4) 0.0440(14) Uani 1 1 d . . .
H18 H 1.3056 0.5330 0.1847 0.053 Uiso 1 1 calc R . .
C19 C 1.1050(6) 0.4263(6) 0.1446(3) 0.0389(11) Uani 1 1 d . . .
H19 H 1.1186 0.4313 0.0982 0.047 Uiso 1 1 calc R . .
C20 C 0.9736(5) 0.3586(4) 0.1626(2) 0.0263(8) Uani 1 1 d . . .
C21 C 0.8502(5) 0.2934(4) 0.1128(2) 0.0267(9) Uani 1 1 d . . .
C22 C 0.8498(5) 0.2790(7) 0.0434(2) 0.0346(9) Uani 1 1 d . . .
H22 H 0.9347 0.3129 0.0232 0.041 Uiso 1 1 calc R . .
C23 C 0.7194(7) 0.2126(6) 0.0038(2) 0.0402(12) Uani 1 1 d . . .
C24 C 0.5932(6) 0.1678(5) 0.0331(2) 0.0343(10) Uani 1 1 d . . .
H24 H 0.5041 0.1254 0.0059 0.041 Uiso 1 1 calc R . .
C25 C 0.6001(5) 0.1864(5) 0.1027(2) 0.0259(8) Uani 1 1 d . . .
C26 C 0.4812(5) 0.1437(4) 0.1448(2) 0.0234(7) Uani 1 1 d . . .
C27 C 0.3398(5) 0.0765(5) 0.1177(2) 0.0317(9) Uani 1 1 d . . .
H27 H 0.3166 0.0532 0.0704 0.038 Uiso 1 1 calc R . .
C28 C 0.2351(6) 0.0445(6) 0.1599(3) 0.0371(11) Uani 1 1 d . . .
H28 H 0.1386 -0.0007 0.1421 0.044 Uiso 1 1 calc R . .
C29 C 0.2711(5) 0.0788(6) 0.2293(3) 0.0345(10) Uani 1 1 d . . .
H29 H 0.1999 0.0580 0.2593 0.041 Uiso 1 1 calc R . .
C30 C 0.4144(5) 0.1445(5) 0.2534(2) 0.0262(8) Uani 1 1 d . . .
H30 H 0.4394 0.1686 0.3005 0.031 Uiso 1 1 calc R . .
O1A O 0.7507(6) 0.2796(8) 0.5475(2) 0.0222(11) Uani 0.50 1 d P . .
O1B O 0.7302(8) 0.1942(8) -0.0622(3) 0.0330(14) Uani 0.50 1 d P . .
O2 O 0.5556(6) 0.4702(5) 0.5922(2) 0.0553(10) Uani 1 1 d D . .
H1W H 0.494(6) 0.411(7) 0.556(2) 0.066 Uiso 1 1 d D . .
H2W H 0.651(5) 0.510(8) 0.577(3) 0.066 Uiso 1 1 d 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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 '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
N5 Ru1 N2 178.4(3) . . ?
N5 Ru1 N4 79.24(14) . . ?
N2 Ru1 N4 101.83(14) . . ?
N5 Ru1 N6 78.67(14) . . ?
N2 Ru1 N6 100.29(13) . . ?
N4 Ru1 N6 157.85(14) . . ?
N5 Ru1 N3 102.51(16) . . ?
N2 Ru1 N3 78.72(19) . . ?
N4 Ru1 N3 90.21(13) . . ?
N6 Ru1 N3 93.02(13) . . ?
N5 Ru1 N1 99.93(16) . . ?
N2 Ru1 N1 78.86(19) . . ?
N4 Ru1 N1 92.57(13) . . ?
N6 Ru1 N1 92.76(13) . . ?
N3 Ru1 N1 157.51(13) . . ?
C1 N1 C5 119.0(4) . . ?
C1 N1 Ru1 127.4(3) . . ?
C5 N1 Ru1 113.6(3) . . ?
C10 N2 C6 121.1(3) . . ?
C10 N2 Ru1 119.4(3) . . ?
C6 N2 Ru1 119.4(4) . . ?
C15 N3 C11 118.7(3) . . ?
C15 N3 Ru1 127.7(3) . . ?
C11 N3 Ru1 113.6(3) . . ?
C16 N4 C20 119.3(4) . . ?
C16 N4 Ru1 127.3(3) . . ?
C20 N4 Ru1 113.3(3) . . ?
C25 N5 C21 121.2(3) . . ?
C25 N5 Ru1 119.9(3) . . ?
C21 N5 Ru1 118.8(3) . . ?
C30 N6 C26 118.7(3) . . ?
C30 N6 Ru1 127.1(3) . . ?
C26 N6 Ru1 114.2(3) . . ?
F1 B1 F3 121.6(6) . . ?
F1 B1 F2 114.4(5) . . ?
F3 B1 F2 116.4(7) . . ?
F1 B1 F4 100.6(7) . . ?
F3 B1 F4 98.0(6) . . ?
F2 B1 F4 99.3(6) . . ?
F8 B2 F6 109.3(5) . . ?
F8 B2 F5 109.3(6) . . ?
F6 B2 F5 107.0(5) . . ?
F8 B2 F7 110.2(5) . . ?
F6 B2 F7 109.9(6) . . ?
F5 B2 F7 111.0(5) . . ?
N1 C1 C2 122.4(4) . . ?
C3 C2 C1 118.8(4) . . ?
C2 C3 C4 119.3(4) . . ?
C5 C4 C3 119.3(4) . . ?
N1 C5 C4 121.2(4) . . ?
N1 C5 C6 115.6(3) . . ?
C4 C5 C6 123.1(4) . . ?
N2 C6 C7 120.9(4) . . ?
N2 C6 C5 112.5(4) . . ?
C7 C6 C5 126.6(4) . . ?
C6 C7 C8 118.6(4) . . ?
O1A C8 C7 115.9(5) . . ?
O1A C8 C9 124.2(5) . . ?
C7 C8 C9 119.9(4) . . ?
C10 C9 C8 118.2(4) . . ?
N2 C10 C9 121.3(4) . . ?
N2 C10 C11 112.9(3) . . ?
C9 C10 C11 125.8(4) . . ?
N3 C11 C12 120.9(4) . . ?
N3 C11 C10 115.2(3) . . ?
C12 C11 C10 123.9(4) . . ?
C13 C12 C11 120.0(4) . . ?
C12 C13 C14 119.2(5) . . ?
C13 C14 C15 119.3(4) . . ?
N3 C15 C14 121.8(4) . . ?
N4 C16 C17 121.7(5) . . ?
C18 C17 C16 119.4(5) . . ?
C17 C18 C19 119.6(4) . . ?
C18 C19 C20 118.9(5) . . ?
N4 C20 C19 121.0(4) . . ?
N4 C20 C21 115.7(3) . . ?
C19 C20 C21 123.2(4) . . ?
N5 C21 C22 121.0(4) . . ?
N5 C21 C20 112.8(3) . . ?
C22 C21 C20 126.2(4) . . ?
C21 C22 C23 117.6(4) . . ?
O1B C23 C24 124.4(6) . . ?
O1B C23 C22 114.6(5) . . ?
C24 C23 C22 121.0(4) . . ?
C25 C24 C23 118.5(4) . . ?
N5 C25 C24 120.6(4) . . ?
N5 C25 C26 111.7(3) . . ?
C24 C25 C26 127.7(4) . . ?
N6 C26 C27 121.3(4) . . ?
N6 C26 C25 115.4(3) . . ?
C27 C26 C25 123.3(4) . . ?
C28 C27 C26 119.4(4) . . ?
C27 C28 C29 119.6(4) . . ?
C28 C29 C30 118.3(4) . . ?
N6 C30 C29 122.6(4) . . ?
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
Ru1 N5 1.981(3) . ?
Ru1 N2 1.989(3) . ?
Ru1 N4 2.073(3) . ?
Ru1 N6 2.077(3) . ?
Ru1 N3 2.081(3) . ?
Ru1 N1 2.090(4) . ?
N1 C1 1.338(5) . ?
N1 C5 1.371(5) . ?
N2 C10 1.338(7) . ?
N2 C6 1.356(6) . ?
N3 C15 1.347(5) . ?
N3 C11 1.373(5) . ?
N4 C16 1.334(6) . ?
N4 C20 1.379(6) . ?
N5 C25 1.354(5) . ?
N5 C21 1.361(5) . ?
N6 C30 1.343(5) . ?
N6 C26 1.361(5) . ?
B1 F1 1.313(8) . ?
B1 F3 1.314(8) . ?
B1 F2 1.355(8) . ?
B1 F4 1.477(10) . ?
B2 F8 1.372(6) . ?
B2 F6 1.374(9) . ?
B2 F5 1.379(7) . ?
B2 F7 1.402(6) . ?
C1 C2 1.393(6) . ?
C2 C3 1.388(7) . ?
C3 C4 1.391(6) . ?
C4 C5 1.388(6) . ?
C5 C6 1.479(5) . ?
C6 C7 1.386(6) . ?
C7 C8 1.394(7) . ?
C8 O1A 1.331(6) . ?
C8 C9 1.408(7) . ?
C9 C10 1.388(5) . ?
C10 C11 1.477(5) . ?
C11 C12 1.388(6) . ?
C12 C13 1.374(7) . ?
C13 C14 1.382(6) . ?
C14 C15 1.392(6) . ?
C16 C17 1.397(6) . ?
C17 C18 1.383(9) . ?
C18 C19 1.389(9) . ?
C19 C20 1.397(6) . ?
C20 C21 1.459(6) . ?
C21 C22 1.385(6) . ?
C22 C23 1.405(8) . ?
C23 O1B 1.339(7) . ?
C23 C24 1.391(7) . ?
C24 C25 1.384(6) . ?
C25 C26 1.489(6) . ?
C26 C27 1.400(6) . ?
C27 C28 1.372(8) . ?
C28 C29 1.395(8) . ?
C29 C30 1.395(6) . ?
