#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:42:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179512 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/09/4340990.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_4340990
loop_
_publ_author_name
'Kulmaczewski, Rafal'
'Shepherd, Helena J.'
'Cespedes, Oscar'
'Halcrow, Malcolm A.'
_publ_section_title
;
 A homologous series of [Fe(H₂Bpz₂)₂(L)]
 spin-crossover complexes with annelated bipyridyl co-ligands.
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9809
_journal_page_last               9817
_journal_paper_doi               10.1021/ic501402q
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C18 H10 N4, C H Cl3'
_chemical_formula_sum            'C19 H11 Cl3 N4'
_chemical_formula_weight         401.67
_chemical_name_systematic
;
Dipyrido[3,2-a:2'3'-c]phenazine chloroform solvate
;
_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   difmap
_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                   9.6126(2)
_cell_length_b                   6.6382(2)
_cell_length_c                   26.5590(6)
_cell_measurement_reflns_used    2932
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.73
_cell_measurement_theta_min      4.87
_cell_volume                     1694.74(7)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0746
_diffrn_reflns_av_sigmaI/netI    0.0497
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            4238
_diffrn_reflns_theta_full        73.93
_diffrn_reflns_theta_max         73.93
_diffrn_reflns_theta_min         4.89
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.987
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.753
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         1787
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0472
_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)+(0.0972P)²+0.0261P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1340
_refine_ls_wR_factor_ref         0.1365
_reflns_number_gt                1665
_reflns_number_total             1787
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501402q_si_009.cif
_cod_data_source_block           rk67b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4340990--4341018.cif.
;
_cod_database_code               4340990
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'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
C1 C 0.8262(2) 0.7500 0.56042(8) 0.0121(4) Uani 1 2 d S
N2 N 0.82568(18) 0.7500 0.61146(7) 0.0142(4) Uani 1 2 d S
C3 C 0.9471(2) 0.7500 0.63485(8) 0.0169(5) Uani 1 2 d S
H3 H 0.944(3) 0.7500 0.6701(12) 0.020 Uiso 1 2 d S
C4 C 1.0759(2) 0.7500 0.61001(9) 0.0183(5) Uani 1 2 d S
H4 H 1.169(3) 0.7500 0.6292(12) 0.022 Uiso 1 2 d S
C5 C 1.0761(2) 0.7500 0.55805(9) 0.0166(5) Uani 1 2 d S
H5 H 1.153(3) 0.7500 0.5413(12) 0.020 Uiso 1 2 d S
C6 C 0.9491(2) 0.7500 0.53219(8) 0.0135(5) Uani 1 2 d S
C7 C 0.6907(2) 0.7500 0.53506(8) 0.0134(4) Uani 1 2 d S
N8 N 0.57704(19) 0.7500 0.56396(7) 0.0186(4) Uani 1 2 d S
C9 C 0.4546(2) 0.7500 0.54179(9) 0.0208(5) Uani 1 2 d S
H9 H 0.380(4) 0.7500 0.5591(12) 0.025 Uiso 1 2 d S
C10 C 0.4352(2) 0.7500 0.48933(9) 0.0202(5) Uani 1 2 d S
H10 H 0.345(3) 0.7500 0.4739(12) 0.024 Uiso 1 2 d S
C11 C 0.5517(2) 0.7500 0.45914(8) 0.0171(5) Uani 1 2 d S
H11 H 0.538(3) 0.7500 0.4239(13) 0.020 Uiso 1 2 d S
C12 C 0.6839(2) 0.7500 0.48187(8) 0.0133(4) Uani 1 2 d S
C13 C 0.9439(2) 0.7500 0.47697(8) 0.0129(4) Uani 1 2 d S
N14 N 1.06256(18) 0.7500 0.45166(7) 0.0148(4) Uani 1 2 d S
C15 C 1.0536(2) 0.7500 0.40049(9) 0.0173(5) Uani 1 2 d S
C16 C 1.1776(2) 0.7500 0.37148(9) 0.0204(5) Uani 1 2 d S
H16 H 1.268(3) 0.7500 0.3878(12) 0.024 Uiso 1 2 d S
C17 C 1.1696(3) 0.7500 0.32002(9) 0.0239(5) Uani 1 2 d S
H17 H 1.252(3) 0.7500 0.2986(13) 0.029 Uiso 1 2 d S
C18 C 1.0388(3) 0.7500 0.29545(9) 0.0254(5) Uani 1 2 d S
H18 H 1.036(4) 0.7500 0.2605(14) 0.030 Uiso 1 2 d S
C19 C 0.9177(3) 0.7500 0.32250(9) 0.0220(5) Uani 1 2 d S
H19 H 0.832(4) 0.7500 0.3078(12) 0.026 Uiso 1 2 d S
C20 C 0.9219(2) 0.7500 0.37591(8) 0.0167(5) Uani 1 2 d S
N21 N 0.80136(19) 0.7500 0.40209(7) 0.0155(4) Uani 1 2 d S
C22 C 0.8118(2) 0.7500 0.45208(8) 0.0135(4) Uani 1 2 d S
C23 C 0.5493(2) 0.7500 0.67830(9) 0.0210(5) Uani 1 2 d S
H23 H 0.614(3) 0.7500 0.6501(12) 0.025 Uiso 1 2 d S
Cl24 Cl 0.63708(7) 0.7500 0.73666(2) 0.0341(2) Uani 1 2 d S
Cl25 Cl 0.44441(5) 0.53302(8) 0.671644(17) 0.0314(2) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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
N2 C1 C6 122.65(18) .
N2 C1 C7 117.12(17) .
C6 C1 C7 120.24(18) .
C3 N2 C1 117.80(18) .
N2 C3 C4 123.9(2) .
N2 C3 H3 116.5(18) .
C4 C3 H3 119.6(18) .
C5 C4 C3 118.10(19) .
C5 C4 H4 119.5(17) .
C3 C4 H4 122.4(17) .
C4 C5 C6 119.31(19) .
C4 C5 H5 121(2) .
C6 C5 H5 119(2) .
C1 C6 C5 118.2(2) .
C1 C6 C13 120.47(18) .
C5 C6 C13 121.32(18) .
N8 C7 C12 122.41(19) .
N8 C7 C1 117.57(18) .
C12 C7 C1 120.02(18) .
C9 N8 C7 118.35(19) .
N8 C9 C10 124.16(19) .
N8 C9 H9 121(2) .
C10 C9 H9 115(2) .
C11 C10 C9 118.01(19) .
C11 C10 H10 119.0(19) .
C9 C10 H10 123.0(19) .
C10 C11 C12 119.0(2) .
C10 C11 H11 117.8(18) .
C12 C11 H11 123.2(18) .
C11 C12 C7 118.09(19) .
C11 C12 C22 121.83(18) .
C7 C12 C22 120.08(18) .
N14 C13 C22 121.98(19) .
N14 C13 C6 118.57(18) .
C22 C13 C6 119.45(17) .
C13 N14 C15 116.88(18) .
N14 C15 C16 119.2(2) .
N14 C15 C20 120.92(19) .
C16 C15 C20 119.8(2) .
C17 C16 C15 119.7(2) .
C17 C16 H16 119.9(19) .
C15 C16 H16 120.4(19) .
C16 C17 C18 120.6(2) .
C16 C17 H17 122.5(19) .
C18 C17 H17 116.9(19) .
C19 C18 C17 120.9(2) .
C19 C18 H18 120(2) .
C17 C18 H18 119(2) .
C18 C19 C20 120.0(2) .
C18 C19 H19 123(2) .
C20 C19 H19 117(2) .
N21 C20 C19 119.3(2) .
N21 C20 C15 121.8(2) .
C19 C20 C15 118.9(2) .
C22 N21 C20 116.63(18) .
N21 C22 C13 121.82(18) .
N21 C22 C12 118.43(18) .
C13 C22 C12 119.74(18) .
Cl24 C23 Cl25 111.15(9) .
Cl25 C23 Cl25 109.19(13) 8_575
Cl24 C23 H23 111.8(19) .
Cl25 C23 H23 106.7(10) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 N2 1.356(3)
C1 C6 1.399(3)
C1 C7 1.467(3)
N2 C3 1.322(3)
C3 C4 1.403(3)
C3 H3 0.94(3)
C4 C5 1.380(3)
C4 H4 1.03(3)
C5 C6 1.400(3)
C5 H5 0.86(3)
C6 C13 1.467(3)
C7 N8 1.335(3)
C7 C12 1.414(3)
N8 C9 1.316(3)
C9 C10 1.406(3)
C9 H9 0.85(3)
C10 C11 1.377(3)
C10 H10 0.96(3)
C11 C12 1.406(3)
C11 H11 0.95(3)
C12 C22 1.462(3)
C13 N14 1.324(3)
C13 C22 1.432(3)
N14 C15 1.362(3)
C15 C16 1.419(3)
C15 C20 1.424(3)
C16 C17 1.369(3)
C16 H16 0.97(3)
C17 C18 1.417(4)
C17 H17 0.97(3)
C18 C19 1.369(3)
C18 H18 0.93(4)
C19 C20 1.419(3)
C19 H19 0.91(4)
C20 N21 1.351(3)
N21 C22 1.332(3)
C23 Cl24 1.765(2)
C23 Cl25 1.7672(14)
C23 H23 0.97(3)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C23 H23 N2 0.97(3) 2.28(3) 3.195(3) 156(3)
C23 H23 N8 0.97(3) 2.31(3) 3.049(3) 132(2)
