#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/96/2019622.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_2019622
loop_
_publ_author_name
'Nyamato, George S.'
'Ojwach, Stephen O.'
'Akerman, Matthew P.'
_publ_section_title
;
 Packing forces in
 dichloridobis(3,5-diphenyl-1H-pyrazole-κN²)cobalt(II)
 dichloromethane hemisolvate
;
_journal_coeditor_code           YP3074
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229614015411
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Co Cl2 (C15 H12 N2)2] , 0.5C H2 Cl2'
_chemical_formula_moiety         'C30 H24 Cl2 Co N4, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C30.5 H25 Cl3 Co N4'
_chemical_formula_weight         612.85
_chemical_name_systematic
;
Dichloridobis(3,5-diphenyl-1H-pyrazole-κN²)cobalt(II)
dichloromethane hemisolvate
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.7980(9)
_cell_length_b                   20.8958(16)
_cell_length_c                   19.2954(15)
_cell_measurement_reflns_used    4835
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      1.8
_cell_volume                     5563.3(7)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2012)'
_computing_data_collection       'APEX2 (Bruker, 2012)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2012)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXL97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Incoatec microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_sigmaI/netI    0.0229
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26832
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.933
_exptl_absorpt_correction_T_max  0.9461
_exptl_absorpt_correction_T_min  0.8354
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2012)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.250
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         5453
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0244
_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)+(0.0229P)²+3.9174P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0609
_reflns_number_gt                4835
_reflns_number_total             5453
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            yp3074sup1.cf
_cod_data_source_block           I
_cod_original_formula_sum        'C30.5 H25 Cl3 Co1 N4'
_cod_database_code               2019622
_cod_database_fobs_code          2019622
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'-x-1/2, y-1/2, z'
'x, -y, z-1/2'
'x-1/2, y-1/2, -z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
C C1 0.32505(12) 0.33872(7) 0.38532(8) 0.0170(3) Uani d . 1 1
H H1 0.3846 0.3530 0.4047 0.020 Uiso calc R 1 1
C C1S 0.5000 0.51886(15) 0.2500 0.0416(8) Uani d S 1 2
C C2 0.28674(12) 0.36961(8) 0.32782(9) 0.0199(4) Uani d . 1 1
H H2 0.3198 0.4052 0.3084 0.024 Uiso calc R 1 1
C C3 0.20017(12) 0.34882(8) 0.29834(9) 0.0204(4) Uani d . 1 1
H H3 0.1740 0.3703 0.2592 0.024 Uiso calc R 1 1
C C4 0.15231(12) 0.29637(8) 0.32656(8) 0.0190(3) Uani d . 1 1
H H4 0.0940 0.2814 0.3061 0.023 Uiso calc R 1 1
C C5 0.18965(11) 0.26579(8) 0.38467(8) 0.0166(3) Uani d . 1 1
H H5 0.1560 0.2304 0.4041 0.020 Uiso calc R 1 1
C C6 0.27641(11) 0.28664(7) 0.41499(8) 0.0142(3) Uani d . 1 1
C C7 0.31432(11) 0.25201(7) 0.47570(8) 0.0139(3) Uani d . 1 1
C C8 0.29079(11) 0.18950(7) 0.49673(8) 0.0157(3) Uani d . 1 1
H H8 0.2457 0.1614 0.4753 0.019 Uiso calc R 1 1
C C9 0.34617(11) 0.17703(7) 0.55457(8) 0.0143(3) Uani d . 1 1
C C10 0.35515(11) 0.11975(7) 0.59828(8) 0.0149(3) Uani d . 1 1
C C11 0.27413(12) 0.08122(7) 0.61126(8) 0.0177(3) Uani d . 1 1
H H11 0.2129 0.0923 0.5922 0.021 Uiso calc R 1 1
C C12 0.28349(13) 0.02673(8) 0.65198(9) 0.0206(4) Uani d . 1 1
H H12 0.2284 0.0007 0.6609 0.025 Uiso calc R 1 1
C C13 0.37299(13) 0.01010(8) 0.67974(9) 0.0215(4) Uani d . 1 1
H H13 0.3790 -0.0273 0.7074 0.026 Uiso calc R 1 1
C C14 0.45366(13) 0.04824(8) 0.66705(9) 0.0207(4) Uani d . 1 1
H H14 0.5148 0.0369 0.6860 0.025 Uiso calc R 1 1
C C15 0.44488(12) 0.10297(8) 0.62664(8) 0.0171(3) Uani d . 1 1
H H15 0.5000 0.1291 0.6183 0.020 Uiso calc R 1 1
C C16 0.27288(12) 0.56116(8) 0.37405(9) 0.0189(3) Uani d . 1 1
H H16 0.3374 0.5460 0.3787 0.023 Uiso calc R 1 1
C C17 0.25198(13) 0.60959(8) 0.32697(9) 0.0215(4) Uani d . 1 1
H H17 0.3024 0.6277 0.2998 0.026 Uiso calc R 1 1
C C18 0.15729(13) 0.63167(8) 0.31952(9) 0.0231(4) Uani d . 1 1
H H18 0.1433 0.6648 0.2873 0.028 Uiso calc R 1 1
C C19 0.08346(12) 0.60546(8) 0.35903(9) 0.0225(4) Uani d . 1 1
H H19 0.0188 0.6202 0.3535 0.027 Uiso calc R 1 1
C C20 0.10401(12) 0.55754(8) 0.40671(9) 0.0184(3) Uani d . 1 1
H H20 0.0534 0.5401 0.4342 0.022 Uiso calc R 1 1
C C21 0.19875(11) 0.53473(7) 0.41458(8) 0.0160(3) Uani d . 1 1
C C22 0.21675(11) 0.48260(7) 0.46387(8) 0.0156(3) Uani d . 1 1
C C23 0.15326(11) 0.43827(7) 0.49217(8) 0.0162(3) Uani d . 1 1
H H23 0.0855 0.4353 0.4839 0.019 Uiso calc R 1 1
C C24 0.20855(11) 0.39889(7) 0.53528(8) 0.0148(3) Uani d . 1 1
C C25 0.17748(11) 0.34307(7) 0.57646(8) 0.0153(3) Uani d . 1 1
C C26 0.09988(12) 0.30532(8) 0.55428(9) 0.0185(3) Uani d . 1 1
H H26 0.0651 0.3169 0.5137 0.022 Uiso calc R 1 1
C C27 0.07335(12) 0.25110(8) 0.59117(9) 0.0235(4) Uani d . 1 1
H H27 0.0203 0.2258 0.5759 0.028 Uiso calc R 1 1
C C28 0.12390(13) 0.23364(8) 0.65022(10) 0.0251(4) Uani d . 1 1
H H28 0.1062 0.1961 0.6749 0.030 Uiso calc R 1 1
C C29 0.20046(13) 0.27114(8) 0.67327(9) 0.0227(4) Uani d . 1 1
H H29 0.2353 0.2592 0.7137 0.027 Uiso calc R 1 1
C C30 0.22614(12) 0.32621(8) 0.63722(9) 0.0192(3) Uani d . 1 1
H H30 0.2771 0.3525 0.6540 0.023 Uiso calc R 1 1
Cl Cl1 0.48310(3) 0.342643(19) 0.65612(2) 0.01995(9) Uani d . 1 1
Cl Cl1S 0.51433(3) 0.47199(2) 0.32554(2) 0.03041(11) Uani d . 1 1
Cl Cl2 0.53993(3) 0.413550(18) 0.48609(2) 0.01836(9) Uani d . 1 1
Co Co1 0.424708(15) 0.366007(10) 0.550060(11) 0.01355(6) Uani d . 1 1
N N1 0.38080(9) 0.27707(6) 0.51942(7) 0.0144(3) Uani d . 1 1
N N2 0.40041(10) 0.22977(6) 0.56598(7) 0.0148(3) Uani d . 1 1
N N3 0.30251(9) 0.41756(6) 0.53376(7) 0.0147(3) Uani d . 1 1
N N4 0.30528(10) 0.46864(6) 0.48989(7) 0.0150(3) Uani d . 1 1
H H1S 0.4408(18) 0.5437(13) 0.2557(15) 0.072(9) Uiso d . 1 1
H H101 0.4319(12) 0.2399(8) 0.6020(10) 0.015(5) Uiso d . 1 1
H H102 0.3583(14) 0.4898(9) 0.4837(10) 0.020(5) Uiso d . 1 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'
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'
H H 0.0000 0.0000 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
C2 C1 C6 . . 120.35(15)
C2 C1 H1 . . 119.8
C6 C1 H1 . . 119.8
Cl1S C1S Cl1S . 3_655 112.68(17)
Cl1S C1S H1S . . 107.2(17)
Cl1S C1S H1S 3_655 . 107.1(17)
C1 C2 C3 . . 120.53(15)
C1 C2 H2 . . 119.7
C3 C2 H2 . . 119.7
C4 C3 C2 . . 119.56(15)
C4 C3 H3 . . 120.2
C2 C3 H3 . . 120.2
C5 C4 C3 . . 120.15(15)
C5 C4 H4 . . 119.9
C3 C4 H4 . . 119.9
C4 C5 C6 . . 120.69(15)
C4 C5 H5 . . 119.7
C6 C5 H5 . . 119.7
C1 C6 C5 . . 118.69(14)
C1 C6 C7 . . 122.44(14)
C5 C6 C7 . . 118.84(14)
N1 C7 C8 . . 109.67(14)
N1 C7 C6 . . 123.16(14)
C8 C7 C6 . . 127.16(14)
C9 C8 C7 . . 106.35(14)
C9 C8 H8 . . 126.8
C7 C8 H8 . . 126.8
N2 C9 C8 . . 106.57(14)
N2 C9 C10 . . 121.64(14)
C8 C9 C10 . . 131.75(14)
C15 C10 C11 . . 119.52(15)
C15 C10 C9 . . 120.23(14)
C11 C10 C9 . . 120.24(14)
C12 C11 C10 . . 119.88(15)
C12 C11 H11 . . 120.1
C10 C11 H11 . . 120.1
C11 C12 C13 . . 120.35(16)
C11 C12 H12 . . 119.8
C13 C12 H12 . . 119.8
C12 C13 C14 . . 120.00(15)
C12 C13 H13 . . 120.0
C14 C13 H13 . . 120.0
C15 C14 C13 . . 120.05(16)
C15 C14 H14 . . 120.0
C13 C14 H14 . . 120.0
C14 C15 C10 . . 120.21(15)
C14 C15 H15 . . 119.9
C10 C15 H15 . . 119.9
C17 C16 C21 . . 120.02(15)
C17 C16 H16 . . 120.0
C21 C16 H16 . . 120.0
C16 C17 C18 . . 120.20(16)
C16 C17 H17 . . 119.9
C18 C17 H17 . . 119.9
C19 C18 C17 . . 120.13(16)
C19 C18 H18 . . 119.9
C17 C18 H18 . . 119.9
C18 C19 C20 . . 119.97(16)
C18 C19 H19 . . 120.0
C20 C19 H19 . . 120.0
C19 C20 C21 . . 120.52(16)
C19 C20 H20 . . 119.7
C21 C20 H20 . . 119.7
C20 C21 C16 . . 119.16(15)
C20 C21 C22 . . 118.76(15)
C16 C21 C22 . . 122.07(14)
N4 C22 C23 . . 106.28(14)
N4 C22 C21 . . 123.61(14)
C23 C22 C21 . . 130.10(15)
C22 C23 C24 . . 106.44(14)
C22 C23 H23 . . 126.8
C24 C23 H23 . . 126.8
N3 C24 C23 . . 109.90(14)
N3 C24 C25 . . 121.17(14)
C23 C24 C25 . . 128.90(14)
C30 C25 C26 . . 118.90(15)
C30 C25 C24 . . 120.80(14)
C26 C25 C24 . . 120.28(15)
C27 C26 C25 . . 120.41(16)
C27 C26 H26 . . 119.8
C25 C26 H26 . . 119.8
C28 C27 C26 . . 120.29(16)
C28 C27 H27 . . 119.9
C26 C27 H27 . . 119.9
C27 C28 C29 . . 119.87(16)
C27 C28 H28 . . 120.1
C29 C28 H28 . . 120.1
C28 C29 C30 . . 120.05(16)
C28 C29 H29 . . 120.0
C30 C29 H29 . . 120.0
C29 C30 C25 . . 120.42(16)
C29 C30 H30 . . 119.8
C25 C30 H30 . . 119.8
N3 Co1 N1 . . 101.08(5)
N3 Co1 Cl2 . . 105.60(4)
N1 Co1 Cl2 . . 116.98(4)
N3 Co1 Cl1 . . 123.64(4)
N1 Co1 Cl1 . . 99.89(4)
Cl2 Co1 Cl1 . . 110.008(17)
C7 N1 N2 . . 105.38(12)
C7 N1 Co1 . . 137.26(11)
N2 N1 Co1 . . 114.22(10)
C9 N2 N1 . . 111.99(13)
C9 N2 H101 . . 128.5(12)
N1 N2 H101 . . 117.6(12)
C24 N3 N4 . . 105.41(13)
C24 N3 Co1 . . 129.83(11)
N4 N3 Co1 . . 119.32(10)
C22 N4 N3 . . 111.97(13)
C22 N4 H102 . . 127.2(12)
N3 N4 H102 . . 120.7(12)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C1 C2 . 1.388(2)
C1 C6 . 1.401(2)
C1 H1 . 0.9500
C1S Cl1S . 1.7671(17)
C1S Cl1S 3_655 1.7671(17)
C1S H1S . 0.97(2)
C2 C3 . 1.393(2)
C2 H2 . 0.9500
C3 C4 . 1.391(2)
C3 H3 . 0.9500
C4 C5 . 1.390(2)
C4 H4 . 0.9500
C5 C6 . 1.402(2)
C5 H5 . 0.9500
C6 C7 . 1.473(2)
C7 N1 . 1.352(2)
C7 C8 . 1.406(2)
C8 C9 . 1.377(2)
C8 H8 . 0.9500
C9 N2 . 1.350(2)
C9 C10 . 1.469(2)
C10 C15 . 1.398(2)
C10 C11 . 1.400(2)
C11 C12 . 1.389(2)
C11 H11 . 0.9500
C12 C13 . 1.390(2)
C12 H12 . 0.9500
C13 C14 . 1.391(3)
C13 H13 . 0.9500
C14 C15 . 1.389(2)
C14 H14 . 0.9500
C15 H15 . 0.9500
C16 C17 . 1.390(2)
C16 C21 . 1.401(2)
C16 H16 . 0.9500
C17 C18 . 1.393(2)
C17 H17 . 0.9500
C18 C19 . 1.385(3)
C18 H18 . 0.9500
C19 C20 . 1.389(2)
C19 H19 . 0.9500
C20 C21 . 1.400(2)
C20 H20 . 0.9500
C21 C22 . 1.467(2)
C22 N4 . 1.353(2)
C22 C23 . 1.387(2)
C23 C24 . 1.397(2)
C23 H23 . 0.9500
C24 N3 . 1.354(2)
C24 C25 . 1.475(2)
C25 C30 . 1.396(2)
C25 C26 . 1.397(2)
C26 C27 . 1.387(2)
C26 H26 . 0.9500
C27 C28 . 1.385(3)
C27 H27 . 0.9500
C28 C29 . 1.388(3)
C28 H28 . 0.9500
C29 C30 . 1.391(2)
C29 H29 . 0.9500
C30 H30 . 0.9500
Cl1 Co1 . 2.2530(5)
Cl2 Co1 . 2.2446(4)
Co1 N3 . 2.0253(13)
Co1 N1 . 2.0422(13)
N1 N2 . 1.3626(18)
N2 H101 . 0.846(18)
N3 N4 . 1.3629(18)
N4 H102 . 0.863(19)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N4 H102 Cl2 5_666 0.86(2) 2.53(2) 3.2920(10) 148(2) yes
