#------------------------------------------------------------------------------
#$Date: 2019-11-17 10:25:09 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229338 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/75/7047551.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_7047551
loop_
_publ_author_name
'Wang, Hongfeng'
'Baldé, Chérif'
'Grosjean, Arnaud'
'Desplanches, Cédric'
'Guionneau, Philippe'
'Chastanet, Guillaume'
_publ_section_title
;
 Seven-coordinated iron(ii) spin-crossover molecules: some learning from
 iron substitution in
 [FeₓMn₁₋ₓ(L₂₂₂N₃O₂)(CN)₂]·H₂O
 solid solutions.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14741
_journal_page_last               14750
_journal_paper_doi               10.1039/c8dt02517g
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         '0.5(H4 O2), C17 H21 Fe0.96 Mn0.04 N5 O2'
_chemical_formula_sum            'C17 H23 Fe0.96 Mn0.04 N5 O3'
_chemical_formula_weight         401.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-08-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-08-31 deposited with the CCDC.
2018-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.269(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.3438(8)
_cell_length_b                   12.0771(7)
_cell_length_c                   10.1378(7)
_cell_measurement_reflns_used    9572
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      1.00
_cell_volume                     1904.2(2)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_data_reduction        DENZO-SMN
_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      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ scans, and ω scans with κ'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0722
_diffrn_reflns_av_unetI/netI     0.1089
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4369
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.045
_diffrn_reflns_theta_min         2.619
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.814
_exptl_absorpt_correction_T_max  0.9374
_exptl_absorpt_correction_T_min  0.9374
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   scalepack
_exptl_crystal_colour            'dark blue'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.968
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         2586
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.1733
_refine_ls_R_factor_gt           0.0784
_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)+(0.0923P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1617
_refine_ls_wR_factor_ref         0.2000
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1210
_reflns_number_total             2586
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt02517g2.cif
_cod_data_source_block           cdhw73aa
_cod_depositor_comments
'Adding full bibliography for 7047551--7047555.cif.'
_cod_database_code               7047551
_shelx_shelxl_version_number     2018/1
_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   0.938
_shelx_estimated_absorpt_t_min   0.938
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Fe1, Mn1}
3. Restrained distances
 H2a-O2
 0.86 with sigma of 0.02
 O2-H2b
 0.86 with sigma of 0.02
 H2a-H2b
 1.39 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(Fe1) = Uanis(Mn1)
5. Others
 Fixed Sof: O2(0.5) H2a(0.5) H2b(0.5) Fe1(0.48) Mn1(0.02)
 Fixed Uiso: H2a(0.13) H2b(0.13)
6.a Secondary CH2 refined with riding coordinates:
 C7(H7a,H7b), C6(H6a,H6b), C8(H8b,H8a)
6.b Me refined with riding coordinates:
 C5(H5a,H5b,H5c)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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_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
O2 O 0.2268(7) -0.1755(10) -0.0577(12) 0.122(3) Uani 0.5 1 d D . . . .
H2A H 0.190(6) -0.151(11) -0.029(13) 0.130 Uiso 0.5 1 d D . . . .
H2B H 0.266(6) -0.211(11) 0.016(9) 0.130 Uiso 0.5 1 d D . . . .
Fe1 Fe 0.500000 0.26187(7) 0.250000 0.0454(4) Uani 0.96 2 d S T P A 1
C9 C 0.4010(3) 0.2777(4) 0.3252(5) 0.0525(11) Uani 1 1 d . . . . .
O1 O 0.44196(19) 0.4192(3) 0.1059(4) 0.0649(9) Uani 1 1 d . . . . .
N1 N 0.500000 0.0863(4) 0.250000 0.0456(12) Uani 1 2 d S T P . .
N2 N 0.4020(2) 0.2071(3) 0.0320(4) 0.0527(9) Uani 1 1 d . . . . .
C4 C 0.3913(3) 0.1041(4) 0.0043(5) 0.0521(11) Uani 1 1 d . . . . .
N3 N 0.3526(3) 0.2854(4) 0.3689(6) 0.0789(14) Uani 1 1 d . . . . .
C2 C 0.4462(3) -0.0822(4) 0.1250(6) 0.0636(13) Uani 1 1 d . . . . .
H2 H 0.410393 -0.119983 0.039809 0.076 Uiso 1 1 calc R . . . .
C3 C 0.4469(2) 0.0316(3) 0.1295(5) 0.0457(10) Uani 1 1 d . . . . .
C5 C 0.3303(3) 0.0532(5) -0.1384(5) 0.0702(14) Uani 1 1 d . . . . .
H5A H 0.334773 -0.026007 -0.130566 0.105 Uiso 1 1 calc R . . . .
H5B H 0.272664 0.075275 -0.160989 0.105 Uiso 1 1 calc R . . . .
H5C H 0.344437 0.077621 -0.215184 0.105 Uiso 1 1 calc R . . . .
C1 C 0.500000 -0.1389(6) 0.250000 0.072(2) Uani 1 2 d S T P . .
H1 H 0.499999 -0.215870 0.250002 0.086 Uiso 1 2 calc RS T P . .
C7 C 0.3574(3) 0.3986(4) -0.0001(6) 0.0744(16) Uani 1 1 d . . . . .
H7A H 0.337581 0.458774 -0.070736 0.089 Uiso 1 1 calc R . . . .
H7B H 0.319468 0.393649 0.046970 0.089 Uiso 1 1 calc R . . . .
C6 C 0.3556(3) 0.2932(4) -0.0761(6) 0.0689(14) Uani 1 1 d . . . . .
H6A H 0.296556 0.270231 -0.134707 0.083 Uiso 1 1 calc R . . . .
H6B H 0.382218 0.303749 -0.141637 0.083 Uiso 1 1 calc R . . . .
C8 C 0.4552(3) 0.5156(4) 0.1906(6) 0.089(2) Uani 1 1 d . . . . .
H8B H 0.414910 0.517870 0.233020 0.107 Uiso 1 1 calc R . . . .
H8A H 0.445784 0.580435 0.128884 0.107 Uiso 1 1 calc R . . . .
Mn1 Mn 0.500000 0.26187(7) 0.250000 0.0454(4) Uani 0.04 2 d S T P A 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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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'
O O 0.0106 0.0060 '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
C9 Fe1 C9 169.9(2) 2_655 .
C9 Fe1 O1 84.12(15) 2_655 .
C9 Fe1 O1 87.65(14) . .
C9 Fe1 O1 87.65(14) 2_655 2_655
C9 Fe1 O1 84.12(15) . 2_655
C9 Fe1 N2 93.05(15) . 2_655
C9 Fe1 N2 89.98(16) . .
C9 Fe1 N2 89.98(16) 2_655 2_655
C9 Fe1 N2 93.05(15) 2_655 .
O1 Fe1 O1 71.12(16) . 2_655
N1 Fe1 C9 95.06(12) . .
N1 Fe1 C9 95.06(12) . 2_655
N1 Fe1 O1 144.44(8) . 2_655
N1 Fe1 O1 144.44(8) . .
N1 Fe1 N2 72.60(10) . .
N1 Fe1 N2 72.60(10) . 2_655
N2 Fe1 O1 142.78(14) . 2_655
N2 Fe1 O1 71.95(12) 2_655 2_655
N2 Fe1 O1 142.79(14) 2_655 .
N2 Fe1 O1 71.95(12) . .
N2 Fe1 N2 145.2(2) 2_655 .
N3 C9 Fe1 177.4(4) . .
N3 C9 Mn1 177.4(4) . .
C7 O1 Fe1 110.4(3) . .
C7 O1 Mn1 110.4(3) . .
C8 O1 Fe1 112.5(3) . .
C8 O1 C7 116.6(4) . .
C8 O1 Mn1 112.5(3) . .
C3 N1 Fe1 119.7(2) 2_655 .
C3 N1 Fe1 119.7(2) . .
C3 N1 C3 120.7(5) . 2_655
C3 N1 Mn1 119.7(2) . .
C3 N1 Mn1 119.7(2) 2_655 .
C4 N2 Fe1 119.1(3) . .
C4 N2 C6 123.4(4) . .
C4 N2 Mn1 119.1(3) . .
C6 N2 Fe1 117.4(3) . .
C6 N2 Mn1 117.4(3) . .
N2 C4 C3 114.2(4) . .
N2 C4 C5 126.0(4) . .
C3 C4 C5 119.8(4) . .
C3 C2 C1 118.3(5) . .
N1 C3 C4 114.4(4) . .
N1 C3 C2 121.1(4) . .
C2 C3 C4 124.4(4) . .
C2 C1 C2 120.5(6) . 2_655
O1 C7 C6 108.9(4) . .
N2 C6 C7 110.0(4) . .
O1 C8 C8 109.0(4) . 2_655
C9 Mn1 C9 169.9(2) 2_655 .
C9 Mn1 O1 87.65(14) 2_655 2_655
C9 Mn1 O1 84.12(15) 2_655 .
C9 Mn1 O1 84.12(15) . 2_655
C9 Mn1 O1 87.65(14) . .
C9 Mn1 N2 89.98(16) . .
C9 Mn1 N2 93.05(15) 2_655 .
C9 Mn1 N2 93.05(15) . 2_655
C9 Mn1 N2 89.98(16) 2_655 2_655
O1 Mn1 O1 71.12(16) . 2_655
N1 Mn1 C9 95.06(12) . .
N1 Mn1 C9 95.06(12) . 2_655
N1 Mn1 O1 144.44(8) . 2_655
N1 Mn1 O1 144.44(8) . .
N1 Mn1 N2 72.60(10) . .
N1 Mn1 N2 72.60(10) . 2_655
N2 Mn1 O1 142.78(14) . 2_655
N2 Mn1 O1 142.79(14) 2_655 .
N2 Mn1 O1 71.95(12) 2_655 2_655
N2 Mn1 O1 71.95(12) . .
N2 Mn1 N2 145.2(2) 2_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 C9 2.173(5) 2_655
Fe1 C9 2.173(5) .
Fe1 O1 2.336(3) 2_655
Fe1 O1 2.336(3) .
Fe1 N1 2.121(5) .
Fe1 N2 2.210(4) 2_655
Fe1 N2 2.210(4) .
C9 N3 1.113(6) .
C9 Mn1 2.173(5) .
O1 C7 1.405(6) .
O1 C8 1.403(6) .
O1 Mn1 2.336(3) .
N1 C3 1.334(4) .
N1 C3 1.334(4) 2_655
N1 Mn1 2.121(5) .
N2 C4 1.272(6) .
N2 C6 1.465(6) .
N2 Mn1 2.210(4) .
C4 C3 1.491(6) .
C4 C5 1.494(6) .
C2 C3 1.376(6) .
C2 C1 1.377(6) .
C7 C6 1.482(7) .
C8 C8 1.486(10) 2_655
