#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/14/7101439.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_7101439
loop_
_publ_author_name
'Stephen Holmes'
'Rodolphe Clerac'
'Dongfeng Li.'
'Sean Parkin'
'Chad Ruschman'
_publ_section_title
;
Syntheses, Structures, and Magnetic Characterization
of Dicyanometalate(II) Building Blocks: [NEt4][(Tp*)MII(CN)2] [MII = Cr,
Co, Ni; Tp* = hydridotris(3,5-diemethylpyrazolyl)borate]
;
_journal_issue                   38
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/b608297a
_journal_year                    2006
_chemical_formula_sum            'C29 H50 B Co N10 O0.5'
_chemical_formula_weight         616.53
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.2557(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9894(2)
_cell_length_b                   13.7890(3)
_cell_length_c                   24.3416(6)
_cell_measurement_reflns_used    7356
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     3347.49(13)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 1994)'
_computing_publication_material
;
SHELX97-2 (Sheldrick, 1997) and local procedures
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90.0(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       'ω scans at fixed χ = 55°'
_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  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0759
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            13593
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    0.549
_exptl_absorpt_correction_T_max  0.8526
_exptl_absorpt_correction_T_min  0.8103
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.756
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         7636
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0769P)²+3.1597P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1503
_refine_ls_wR_factor_ref         0.1718
_reflns_number_gt                4767
_reflns_number_total             7636
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b608297a.txt
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C29 H50 B Co N10 O0.50'
_cod_database_code               7101439
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_assembly
_atom_site_disorder_group
Co1 Co 0.36863(4) 1.00049(3) 0.165525(16) 0.01917(14) Uani 1 1 d . . .
B1 B 0.4063(4) 0.8316(3) 0.08540(15) 0.0230(8) Uani 1 1 d . . .
H1 H 0.4225 0.7767 0.0598 0.028 Uiso 1 1 calc R . .
N1 N 0.4201(3) 0.8668(2) 0.18689(10) 0.0220(6) Uani 1 1 d . . .
N2 N 0.4282(3) 0.79864(19) 0.14576(10) 0.0220(6) Uani 1 1 d . . .
N3 N 0.5084(3) 0.99414(19) 0.11184(10) 0.0192(6) Uani 1 1 d . . .
N4 N 0.5063(3) 0.91484(19) 0.07687(10) 0.0205(6) Uani 1 1 d . . .
N5 N 0.2275(3) 0.95064(19) 0.10480(10) 0.0204(6) Uani 1 1 d . . .
N6 N 0.2631(3) 0.86993(19) 0.07601(10) 0.0200(6) Uani 1 1 d . . .
N7 N 0.3107(3) 1.2143(2) 0.14158(11) 0.0267(7) Uani 1 1 d . . .
N8 N 0.1772(3) 1.0098(2) 0.25850(12) 0.0288(7) Uani 1 1 d . . .
C1 C 0.4649(4) 0.8749(3) 0.28826(14) 0.0373(9) Uani 1 1 d . . .
H1A H 0.5018 0.9399 0.2833 0.056 Uiso 1 1 calc R . .
H1B H 0.5230 0.8388 0.3149 0.056 Uiso 1 1 calc R . .
H1C H 0.3749 0.8802 0.3020 0.056 Uiso 1 1 calc R . .
C2 C 0.4573(3) 0.8226(3) 0.23447(13) 0.0276(8) Uani 1 1 d . . .
C3 C 0.4904(4) 0.7261(3) 0.22392(14) 0.0303(8) Uani 1 1 d . . .
H3A H 0.5208 0.6789 0.2502 0.036 Uiso 1 1 calc R . .
C4 C 0.4702(3) 0.7129(2) 0.16818(14) 0.0252(8) Uani 1 1 d . . .
C5 C 0.4883(4) 0.6239(3) 0.13449(15) 0.0359(9) Uani 1 1 d . . .
H5A H 0.5294 0.6414 0.1003 0.054 Uiso 1 1 calc R . .
H5B H 0.4008 0.5937 0.1258 0.054 Uiso 1 1 calc R . .
H5C H 0.5465 0.5781 0.1553 0.054 Uiso 1 1 calc R . .
C6 C 0.6435(3) 1.1428(2) 0.12749(14) 0.0264(8) Uani 1 1 d . . .
H6A H 0.6267 1.1351 0.1665 0.040 Uiso 1 1 calc R . .
H6B H 0.5875 1.1953 0.1118 0.040 Uiso 1 1 calc R . .
H6C H 0.7382 1.1584 0.1237 0.040 Uiso 1 1 calc R . .
C7 C 0.6101(3) 1.0509(2) 0.09782(13) 0.0225(7) Uani 1 1 d . . .
C8 C 0.6726(3) 1.0088(2) 0.05384(13) 0.0224(7) Uani 1 1 d . . .
H8A H 0.7470 1.0341 0.0359 0.027 Uiso 1 1 calc R . .
C9 C 0.6055(3) 0.9236(2) 0.04152(12) 0.0207(7) Uani 1 1 d . . .
C10 C 0.6297(3) 0.8509(3) -0.00263(13) 0.0258(8) Uani 1 1 d . . .
H10A H 0.5448 0.8360 -0.0230 0.039 Uiso 1 1 calc R . .
H10B H 0.6671 0.7915 0.0142 0.039 Uiso 1 1 calc R . .
H10C H 0.6931 0.8778 -0.0279 0.039 Uiso 1 1 calc R . .
C11 C 0.0339(3) 1.0612(2) 0.10842(14) 0.0257(8) Uani 1 1 d . . .
H11A H 0.0521 1.0657 0.1483 0.039 Uiso 1 1 calc R . .
H11B H -0.0629 1.0548 0.1002 0.039 Uiso 1 1 calc R . .
H11C H 0.0665 1.1198 0.0908 0.039 Uiso 1 1 calc R . .
C12 C 0.1034(3) 0.9749(2) 0.08707(13) 0.0211(7) Uani 1 1 d . . .
C13 C 0.0572(3) 0.9085(2) 0.04627(13) 0.0231(7) Uani 1 1 d . . .
H13A H -0.0278 0.9088 0.0267 0.028 Uiso 1 1 calc R . .
C14 C 0.1597(3) 0.8432(2) 0.04040(13) 0.0233(7) Uani 1 1 d . . .
C15 C 0.1683(4) 0.7577(3) 0.00331(14) 0.0312(8) Uani 1 1 d . . .
H15A H 0.2485 0.7633 -0.0178 0.047 Uiso 1 1 calc R . .
H15B H 0.0884 0.7555 -0.0220 0.047 Uiso 1 1 calc R . .
H15C H 0.1735 0.6982 0.0253 0.047 Uiso 1 1 calc R . .
C16 C 0.3360(3) 1.1345(3) 0.15130(13) 0.0225(7) Uani 1 1 d . . .
C17 C 0.2513(3) 1.0079(2) 0.22373(13) 0.0226(7) Uani 1 1 d . . .
N9 N 0.9387(3) 0.7762(2) 0.20817(12) 0.0317(7) Uani 1 1 d . . .
C18 C 0.7787(5) 0.9185(4) 0.2078(3) 0.0718(17) Uani 1 1 d . . .
H18A H 0.7700 0.9869 0.1972 0.108 Uiso 1 1 calc R . .
H18B H 0.7648 0.9118 0.2471 0.108 Uiso 1 1 calc R . .
H18C H 0.7115 0.8801 0.1866 0.108 Uiso 1 1 calc R . .
C19 C 0.9161(4) 0.8831(3) 0.19633(17) 0.0427(10) Uani 1 1 d . . .
H19A H 0.9830 0.9211 0.2189 0.051 Uiso 1 1 calc R . .
H19B H 0.9319 0.8955 0.1572 0.051 Uiso 1 1 calc R . .
C20 C 1.0086(5) 0.8029(3) 0.30923(17) 0.0545(13) Uani 1 1 d . . .
H20A H 0.9832 0.7865 0.3464 0.082 Uiso 1 1 calc R . .
H20B H 1.0016 0.8731 0.3037 0.082 Uiso 1 1 calc R . .
H20C H 1.1012 0.7822 0.3047 0.082 Uiso 1 1 calc R . .
C21 C 0.9160(4) 0.7516(3) 0.26741(15) 0.0369(9) Uani 1 1 d . . .
H21A H 0.9268 0.6808 0.2725 0.044 Uiso 1 1 calc R . .
H21B H 0.8222 0.7681 0.2749 0.044 Uiso 1 1 calc R . .
C22 C 1.1287(5) 0.6527(4) 0.2092(3) 0.0805(18) Uani 1 1 d . . .
H22A H 1.2239 0.6457 0.2022 0.121 Uiso 1 1 calc R . .
H22B H 1.0760 0.6061 0.1865 0.121 Uiso 1 1 calc R . .
H22C H 1.1159 0.6402 0.2482 0.121 Uiso 1 1 calc R . .
C23 C 1.0829(4) 0.7551(4) 0.19469(18) 0.0501(12) Uani 1 1 d . . .
H23A H 1.0919 0.7658 0.1549 0.060 Uiso 1 1 calc R . .
H23B H 1.1428 0.8017 0.2149 0.060 Uiso 1 1 calc R . .
C24 C 0.8444(5) 0.7294(4) 0.11136(17) 0.0638(15) Uani 1 1 d . . .
H24A H 0.7850 0.6822 0.0922 0.096 Uiso 1 1 calc R . .
H24B H 0.9361 0.7205 0.0999 0.096 Uiso 1 1 calc R . .
H24C H 0.8139 0.7952 0.1021 0.096 Uiso 1 1 calc R . .
C25 C 0.8416(4) 0.7139(3) 0.17346(16) 0.0418(10) Uani 1 1 d . . .
H25A H 0.7496 0.7270 0.1847 0.050 Uiso 1 1 calc R . .
H25B H 0.8617 0.6449 0.1816 0.050 Uiso 1 1 calc R . .
N10 N 0.0905(8) 0.5401(6) 0.0791(3) 0.138(2) Uani 1 1 d U . .
C26 C 0.1314(9) 0.4664(5) 0.0645(3) 0.106(3) Uani 1 1 d . . .
C27 C 0.1794(8) 0.3786(4) 0.0467(3) 0.095(2) Uani 1 1 d . . .
H27A H 0.1292 0.3593 0.0127 0.143 Uiso 1 1 calc R . .
H27B H 0.1686 0.3292 0.0750 0.143 Uiso 1 1 calc R . .
H27C H 0.2746 0.3851 0.0396 0.143 Uiso 1 1 calc R . .
O1 O 0.5706(5) 0.5003(4) 0.0144(2) 0.1033(17) Uani 0.50 1 d PU . 1
C28 C 0.7477(12) 0.4367(6) 0.0857(4) 0.069(3) Uani 0.50 1 d PU A 1
H28A H 0.7731 0.3775 0.1060 0.103 Uiso 0.50 1 calc PR A 1
H28B H 0.7438 0.4911 0.1114 0.103 Uiso 0.50 1 calc PR A 1
H28C H 0.8143 0.4504 0.0587 0.103 Uiso 0.50 1 calc PR A 1
C29 C 0.6041(18) 0.4219(17) 0.0546(9) 0.086(3) Uani 0.50 1 d PU A 1
H29A H 0.6026 0.3589 0.0351 0.104 Uiso 0.50 1 calc PR A 1
H29B H 0.5348 0.4198 0.0821 0.104 Uiso 0.50 1 calc PR A 1
C30 C 0.5518(14) 0.4114(15) 0.0509(8) 0.069(4) Uani 0.50 1 d PU B 2
H30A H 0.6358 0.3975 0.0722 0.104 Uiso 0.50 1 calc PR B 2
H30B H 0.5267 0.3554 0.0278 0.104 Uiso 0.50 1 calc PR B 2
H30C H 0.4808 0.4244 0.0761 0.104 Uiso 0.50 1 calc PR B 2
C31 C 0.5706(5) 0.5003(4) 0.0144(2) 0.1033(17) Uani 0.50 1 d PU . 2
H31A H 0.6419 0.4906 -0.0117 0.124 Uiso 0.50 1 calc PR . 2
H31B H 0.5884 0.5601 0.0361 0.124 Uiso 0.50 1 calc PR . 2
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'
B B 0.0013 0.0007 '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'
Co Co 0.3494 0.9721 '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_3
C17 Co1 C16 88.66(13) .
C17 Co1 N3 173.09(12) .
C16 Co1 N3 92.46(12) .
C17 Co1 N1 90.94(12) .
C16 Co1 N1 172.95(12) .
N3 Co1 N1 87.11(11) .
C17 Co1 N5 97.19(12) .
C16 Co1 N5 95.07(12) .
N3 Co1 N5 89.51(10) .
N1 Co1 N5 91.96(11) .
N6 B1 N2 109.0(3) .
N6 B1 N4 109.3(3) .
N2 B1 N4 106.9(3) .
C2 N1 N2 107.0(3) .
C2 N1 Co1 134.9(2) .
N2 N1 Co1 118.05(19) .
C4 N2 N1 109.3(2) .
C4 N2 B1 131.6(3) .
N1 N2 B1 118.7(3) .
C7 N3 N4 106.8(3) .
C7 N3 Co1 136.0(2) .
N4 N3 Co1 117.19(19) .
C9 N4 N3 109.5(3) .
C9 N4 B1 130.9(3) .
N3 N4 B1 119.4(3) .
C12 N5 N6 107.6(2) .
C12 N5 Co1 136.2(2) .
N6 N5 Co1 116.20(19) .
C14 N6 N5 109.6(3) .
C14 N6 B1 132.1(3) .
N5 N6 B1 118.1(2) .
N1 C2 C3 109.3(3) .
N1 C2 C1 122.4(3) .
C3 C2 C1 128.3(3) .
C4 C3 C2 106.5(3) .
N2 C4 C3 107.9(3) .
N2 C4 C5 122.6(3) .
C3 C4 C5 129.5(3) .
N3 C7 C8 109.3(3) .
N3 C7 C6 121.7(3) .
C8 C7 C6 129.0(3) .
C9 C8 C7 106.8(3) .
N4 C9 C8 107.6(3) .
N4 C9 C10 123.3(3) .
C8 C9 C10 129.1(3) .
N5 C12 C13 109.1(3) .
N5 C12 C11 122.2(3) .
C13 C12 C11 128.7(3) .
C14 C13 C12 106.4(3) .
N6 C14 C13 107.3(3) .
N6 C14 C15 122.2(3) .
C13 C14 C15 130.4(3) .
N7 C16 Co1 176.9(3) .
N8 C17 Co1 177.6(3) .
C21 N9 C25 106.2(3) .
C21 N9 C19 111.7(3) .
C25 N9 C19 111.2(3) .
C21 N9 C23 111.0(3) .
C25 N9 C23 110.8(3) .
C19 N9 C23 106.1(3) .
C18 C19 N9 114.2(3) .
N9 C21 C20 114.7(3) .
C22 C23 N9 113.8(4) .
N9 C25 C24 115.1(3) .
N10 C26 C27 179.5(10) .
C29 O1 O1 117.6(10) 3_665
O1 C29 C28 112.5(14) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 C17 1.892(3) .
Co1 C16 1.904(4) .
Co1 N3 1.968(3) .
Co1 N1 1.975(3) .
Co1 N5 2.100(3) .
B1 N6 1.530(5) .
B1 N2 1.542(4) .
B1 N4 1.544(5) .
N1 C2 1.342(4) .
N1 N2 1.379(4) .
N2 C4 1.358(4) .
N3 C7 1.342(4) .
N3 N4 1.385(4) .
N4 C9 1.354(4) .
N5 C12 1.331(4) .
N5 N6 1.373(4) .
N6 C14 1.361(4) .
N7 C16 1.151(4) .
N8 C17 1.156(4) .
C1 C2 1.493(5) .
C2 C3 1.399(5) .
C3 C4 1.372(5) .
C4 C5 1.493(5) .
C6 C7 1.487(5) .
C7 C8 1.395(4) .
C8 C9 1.377(5) .
C9 C10 1.499(4) .
C11 C12 1.486(5) .
C12 C13 1.409(4) .
C13 C14 1.378(5) .
C14 C15 1.489(5) .
N9 C21 1.511(4) .
N9 C25 1.516(5) .
N9 C19 1.517(5) .
N9 C23 1.523(5) .
C18 C19 1.498(6) .
C20 C21 1.512(6) .
C22 C23 1.520(7) .
C24 C25 1.529(5) .
N10 C26 1.159(9) .
C26 C27 1.380(8) .
O1 C29 1.48(2) .
O1 O1 1.539(12) 3_665
C28 C29 1.60(2) .
