#------------------------------------------------------------------------------
#$Date: 2020-05-05 16:18:23 +0300 (Tue, 05 May 2020) $
#$Revision: 251616 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/38/7703846.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_7703846
loop_
_publ_author_name
'Hiiuk, Volodymyr M.'
'Shova, Sergiu'
'Rotaru, Aurelian'
'Golub, Alexander A.'
'Fritsky, Igor O.'
'Gural'skiy, Il'ya A.'
_publ_section_title
;
 Spin crossover in 2D iron(ii) phthalazine cyanometallic complexes.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5302
_journal_page_last               5311
_journal_paper_doi               10.1039/d0dt00783h
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C20 H12 Fe N8 Pd'
_chemical_formula_sum            'C20 H12 Fe N8 Pd'
_chemical_formula_weight         526.63
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-11-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-02 deposited with the CCDC.	2020-03-24 downloaded from the CCDC.
;
_cell_angle_alpha                71.858(6)
_cell_angle_beta                 69.586(6)
_cell_angle_gamma                89.943(5)
_cell_formula_units_Z            1
_cell_length_a                   7.2433(4)
_cell_length_b                   7.4455(4)
_cell_length_c                   10.4263(9)
_cell_measurement_reflns_used    4651
_cell_measurement_temperature    260
_cell_measurement_theta_max      29.3750
_cell_measurement_theta_min      2.1980
_cell_volume                     497.11(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      260
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.875
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.875
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7465
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.875
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.438
_diffrn_reflns_theta_min         2.209
_exptl_absorpt_coefficient_mu    1.658
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.759
_exptl_crystal_description       block
_exptl_crystal_F_000             260
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.218
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2416
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0573P)²+1.0695P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1134
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2285
_reflns_number_total             2416
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt00783h2.cif
_cod_data_source_block           new
_cod_depositor_comments
'Adding full bibliography for 7703844--7703847.cif.'
_cod_database_code               7703846
_shelx_shelxl_version_number     2017/1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.922
_shelx_estimated_absorpt_t_min   0.852
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C10(H10), C8(H8), C7(H7), C6(H6), C5(H5)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.000000 0.500000 0.000000 0.01664(14) Uani 1 2 d S T P . .
Fe1 Fe -0.500000 0.000000 0.000000 0.01800(18) Uani 1 2 d S T P . .
N1 N -0.2621(5) 0.2169(5) -0.0515(4) 0.0300(8) Uani 1 1 d . . . . .
N2 N 0.2888(5) 0.1952(5) 0.0436(4) 0.0282(7) Uani 1 1 d . . . . .
N3 N -0.4893(5) 0.0973(5) -0.2257(4) 0.0286(7) Uani 1 1 d . . . . .
N4 N -0.3065(6) 0.1080(6) -0.3305(4) 0.0371(9) Uani 1 1 d . . . . .
C1 C -0.1619(6) 0.3208(5) -0.0379(4) 0.0225(7) Uani 1 1 d . . . . .
C2 C 0.1798(6) 0.3031(6) 0.0345(4) 0.0238(8) Uani 1 1 d . . . . .
C9 C -0.6321(7) 0.2228(7) -0.4067(5) 0.0314(9) Uani 1 1 d . . . . .
C3 C -0.2901(7) 0.1720(8) -0.4652(5) 0.0405(11) Uani 1 1 d . . . . .
H3 H -0.166482 0.175825 -0.535054 0.049 Uiso 1 1 calc R . . . .
C10 C -0.6417(7) 0.1467(7) -0.2615(5) 0.0318(9) Uani 1 1 d . . . . .
H10 H -0.764280 0.131183 -0.187411 0.038 Uiso 1 1 calc R . . . .
C4 C -0.4454(7) 0.2368(7) -0.5148(5) 0.0346(10) Uani 1 1 d . . . . .
C8 C -0.7932(8) 0.2847(8) -0.4463(6) 0.0431(12) Uani 1 1 d . . . . .
H8 H -0.918531 0.272040 -0.375835 0.052 Uiso 1 1 calc R . . . .
C7 C -0.7632(9) 0.3646(8) -0.5911(7) 0.0506(14) Uani 1 1 d . . . . .
H7 H -0.868066 0.411138 -0.618274 0.061 Uiso 1 1 calc R . . . .
C6 C -0.5782(10) 0.3768(9) -0.6975(6) 0.0539(15) Uani 1 1 d . . . . .
H6 H -0.562154 0.429407 -0.794748 0.065 Uiso 1 1 calc R . . . .
C5 C -0.4204(8) 0.3135(8) -0.6625(6) 0.0481(13) Uani 1 1 d . . . . .
H5 H -0.297975 0.320650 -0.734648 0.058 Uiso 1 1 calc R . . . .
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'
Fe Fe 0.3463 0.8444 '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'
Pd Pd -0.9988 1.0072 '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
C1 Pd1 C1 180.0 . 2_565 ?
C1 Pd1 C2 90.15(15) . . ?
C1 Pd1 C2 90.15(15) 2_565 2_565 ?
C1 Pd1 C2 89.85(15) 2_565 . ?
C1 Pd1 C2 89.85(15) . 2_565 ?
C2 Pd1 C2 180.0 . 2_565 ?
N1 Fe1 N1 180.0 . 2_455 ?
N1 Fe1 N3 91.97(14) . . ?
N1 Fe1 N3 91.97(14) 2_455 2_455 ?
N1 Fe1 N3 88.03(14) 2_455 . ?
N1 Fe1 N3 88.03(14) . 2_455 ?
N2 Fe1 N1 90.15(14) 1_455 2_455 ?
N2 Fe1 N1 89.85(14) 2 2_455 ?
N2 Fe1 N1 90.15(14) 2 . ?
N2 Fe1 N1 89.85(14) 1_455 . ?
N2 Fe1 N2 180.00(19) 2 1_455 ?
N2 Fe1 N3 92.04(14) 2 . ?
N2 Fe1 N3 92.04(14) 1_455 2_455 ?
N2 Fe1 N3 87.96(14) 2 2_455 ?
N2 Fe1 N3 87.96(14) 1_455 . ?
N3 Fe1 N3 180.0 . 2_455 ?
C1 N1 Fe1 160.7(3) . . ?
C2 N2 Fe1 163.8(3) . 1_655 ?
N4 N3 Fe1 115.6(3) . . ?
C10 N3 Fe1 123.8(3) . . ?
C10 N3 N4 120.6(4) . . ?
C3 N4 N3 118.1(4) . . ?
N1 C1 Pd1 176.0(4) . . ?
N2 C2 Pd1 175.0(4) . . ?
C4 C9 C10 115.9(4) . . ?
C8 C9 C10 124.4(4) . . ?
C8 C9 C4 119.7(4) . . ?
N4 C3 H3 117.3 . . ?
N4 C3 C4 125.3(5) . . ?
C4 C3 H3 117.3 . . ?
N3 C10 C9 124.0(4) . . ?
N3 C10 H10 118.0 . . ?
C9 C10 H10 118.0 . . ?
C9 C4 C3 116.1(4) . . ?
C9 C4 C5 120.1(5) . . ?
C5 C4 C3 123.9(5) . . ?
C9 C8 H8 120.5 . . ?
C7 C8 C9 119.0(5) . . ?
C7 C8 H8 120.5 . . ?
C8 C7 H7 119.6 . . ?
C8 C7 C6 120.9(5) . . ?
C6 C7 H7 119.6 . . ?
C7 C6 H6 119.3 . . ?
C5 C6 C7 121.4(5) . . ?
C5 C6 H6 119.3 . . ?
C4 C5 H5 120.6 . . ?
C6 C5 C4 118.8(5) . . ?
C6 C5 H5 120.6 . . ?
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
Pd1 C1 1.991(4) . ?
Pd1 C1 1.991(4) 2_565 ?
Pd1 C2 1.992(4) 2_565 ?
Pd1 C2 1.992(4) . ?
Fe1 N1 2.164(3) 2_455 ?
Fe1 N1 2.164(3) . ?
Fe1 N2 2.140(3) 1_455 ?
Fe1 N2 2.140(3) 2 ?
Fe1 N3 2.209(4) . ?
Fe1 N3 2.209(4) 2_455 ?
N1 C1 1.135(5) . ?
N2 C2 1.132(5) . ?
N3 N4 1.375(5) . ?
N3 C10 1.302(5) . ?
N4 C3 1.296(6) . ?
C9 C10 1.418(6) . ?
C9 C4 1.405(7) . ?
C9 C8 1.400(6) . ?
C3 H3 0.9300 . ?
C3 C4 1.420(7) . ?
C10 H10 0.9300 . ?
C4 C5 1.410(7) . ?
C8 H8 0.9300 . ?
C8 C7 1.376(7) . ?
C7 H7 0.9300 . ?
C7 C6 1.391(9) . ?
C6 H6 0.9300 . ?
C6 C5 1.358(8) . ?
C5 H5 0.9300 . ?
