#------------------------------------------------------------------------------
#$Date: 2019-03-05 09:52:05 +0100 (mar 05 de mar de 2019) $
#$Revision: 213973 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/21/7012133.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_7012133
loop_
_publ_author_name
'Hitchcock, Peter B.'
'Handley, Darren A.'
'Huei Lee, Ting'
'Jeffery Leigh, G.'
_publ_section_title
;
 Anomalous reactions of the diamine Me2NCH2NMe2 with nickel(ii) and
 cobalt(ii)
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4720
_journal_paper_doi               10.1039/b207818j
_journal_year                    2002
_chemical_formula_sum            'C7 H19 Cl2 Co N3'
_chemical_formula_weight         275.08
_chemical_name_common            '[CoCl2(Me2NCH2NMeCH2NMe2)]'
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.079(3)
_cell_length_b                   10.960(3)
_cell_length_c                   9.231(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      7
_cell_volume                     1222.1(6)
_computing_cell_refinement       'Enraf-Nonius CAD4'
_computing_data_collection       'Enraf-Nonius CAD4'
_computing_molecular_graphics    'CAMERON (Watkin and Pearce,1993)'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_method       ω--2θ
_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  0.0533
_diffrn_reflns_av_sigmaI/netI    0.0454
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5563
_diffrn_reflns_theta_full        27.97
_diffrn_reflns_theta_max         27.97
_diffrn_reflns_theta_min         2.78
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.806
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    ' refined '
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         1547
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0187P)²+0.1466P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0658
_reflns_number_gt                1161
_reflns_number_total             1547
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b207818j.txt
_cod_data_source_block           feb999
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7012133
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x+1/2, -y, z+1/2'
'-x, -y, -z'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'
'x-1/2, y, -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
Co Co 0.65471(4) 0.7500 0.12291(5) 0.01845(12) Uani 1 2 d S . .
Cl1 Cl 0.80988(7) 0.7500 -0.01053(9) 0.0285(2) Uani 1 2 d S . .
Cl2 Cl 0.49538(7) 0.7500 0.00052(9) 0.0282(2) Uani 1 2 d S . .
N1 N 0.65285(16) 0.60356(16) 0.2646(2) 0.0199(4) Uani 1 1 d . . .
N2 N 0.6327(2) 0.7500 0.4596(3) 0.0226(6) Uani 1 2 d S . .
C1 C 0.6363(4) 0.7500 0.6174(4) 0.0417(10) Uani 1 2 d S . .
H1A H 0.564(4) 0.7500 0.668(5) 0.062(15) Uiso 1 2 d S . .
H1B H 0.678(2) 0.680(3) 0.650(3) 0.056(10) Uiso 1 1 d . . .
C2 C 0.5895(2) 0.6393(2) 0.3961(3) 0.0244(5) Uani 1 1 d . . .
H2B H 0.594(2) 0.575(3) 0.472(3) 0.034(7) Uiso 1 1 d . . .
H2A H 0.515(2) 0.646(2) 0.369(3) 0.033(7) Uiso 1 1 d . . .
C3 C 0.7672(2) 0.5682(2) 0.3056(3) 0.0258(5) Uani 1 1 d . . .
H3A H 0.768(2) 0.497(2) 0.364(3) 0.030(7) Uiso 1 1 d . . .
H3B H 0.808(2) 0.548(2) 0.218(3) 0.027(7) Uiso 1 1 d . . .
H3C H 0.798(2) 0.631(2) 0.358(3) 0.028(7) Uiso 1 1 d . . .
C4 C 0.5971(2) 0.4970(2) 0.1975(3) 0.0266(5) Uani 1 1 d . . .
H4C H 0.520(2) 0.515(2) 0.170(3) 0.037(8) Uiso 1 1 d . . .
H4A H 0.594(2) 0.429(2) 0.265(3) 0.029(7) Uiso 1 1 d . . .
H4B H 0.635(2) 0.475(2) 0.111(3) 0.029(7) Uiso 1 1 d . . .
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
Co 0.0184(2) 0.0184(2) 0.0186(2) 0.000 -0.00028(18) 0.000
Cl1 0.0253(4) 0.0311(5) 0.0292(5) 0.000 0.0073(3) 0.000
Cl2 0.0248(4) 0.0298(5) 0.0300(5) 0.000 -0.0095(3) 0.000
N1 0.0183(9) 0.0186(9) 0.0228(9) 0.0002(8) -0.0004(8) -0.0002(8)
N2 0.0279(16) 0.0208(14) 0.0190(14) 0.000 0.0010(11) 0.000
C1 0.069(3) 0.033(2) 0.0237(19) 0.000 -0.003(2) 0.000
C2 0.0254(13) 0.0250(12) 0.0227(12) -0.0011(10) 0.0025(10) -0.0036(10)
C3 0.0239(12) 0.0228(13) 0.0306(14) 0.0021(11) -0.0050(11) 0.0029(10)
C4 0.0313(14) 0.0200(12) 0.0284(12) -0.0027(10) -0.0007(12) -0.0050(10)
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'
Cl Cl 0.1484 0.1585 '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'
N N 0.0061 0.0033 '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
N1 Co N1 101.64(10) 7_575 . ?
N1 Co Cl2 108.09(6) 7_575 . ?
N1 Co Cl2 108.09(6) . . ?
N1 Co Cl1 110.85(6) 7_575 . ?
N1 Co Cl1 110.85(6) . . ?
Cl2 Co Cl1 116.27(4) . . ?
C4 N1 C3 108.84(19) . . ?
C4 N1 C2 108.35(18) . . ?
C3 N1 C2 109.82(19) . . ?
C4 N1 Co 110.56(15) . . ?
C3 N1 Co 110.73(15) . . ?
C2 N1 Co 108.50(14) . . ?
C2 N2 C2 114.2(3) . 7_575 ?
C2 N2 C1 114.58(17) . . ?
C2 N2 C1 114.58(17) 7_575 . ?
N2 C2 N1 111.5(2) . . ?
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
Co N1 2.0706(18) 7_575 ?
Co N1 2.0706(18) . ?
Co Cl2 2.2317(10) . ?
Co Cl1 2.2429(11) . ?
N1 C4 1.484(3) . ?
N1 C3 1.484(3) . ?
N1 C2 1.488(3) . ?
N2 C2 1.445(3) . ?
N2 C2 1.445(3) 7_575 ?
N2 C1 1.457(5) . ?
