A luminescent Pt2Fe spin crossover complex.
Schäfer, Bernhard; Bauer, Thomas; Faus, Isabelle; Wolny, Juliusz A.; Dahms, Fabian; Fuhr, Olaf; Lebedkin, Sergei; Wille, Hans-Christian; Schlage, Kai; Chevalier, Katharina; Rupp, Fabian; Diller, Rolf; Schünemann, Volker; Kappes, Manfred M.; Ruben, Mario; Dalton transactions (Cambridge, England : 2003) 46 (2017) 2289–2302; doi:10.1039/c6dt04360g

data_7041876
_publ_section_title
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 A luminescent Pt2Fe spin crossover complex.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2289
_journal_page_last               2302
_journal_paper_doi               10.1039/c6dt04360g
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C80 H84 Fe N16 Pt2, 4(B F4), 3.5(C H2 Cl2)'
_chemical_formula_sum            'C83.5 H91 B4 Cl7 F16 Fe N16 Pt2'
_chemical_formula_weight         2360.14
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-12-21
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2016-12-22 deposited with the CCDC.
2017-01-12 downloaded from the CCDC.
;
_cell_angle_alpha                92.483(2)
_cell_angle_beta                 114.560(2)
_cell_angle_gamma                90.524(2)
_cell_formula_units_Z            2
_cell_length_a                   16.3344(3)
_cell_length_b                   17.2029(4)
_cell_length_c                   18.5945(4)
_cell_measurement_reflns_used    30898
_cell_measurement_temperature    180.15
_cell_measurement_theta_max      26.10
_cell_measurement_theta_min      1.40
_cell_volume                     4745.73(19)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      180.15
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_unetI/netI     0.0643
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            36901
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.632
_diffrn_reflns_theta_min         1.399
_diffrn_source                   'Bruker rotating anode'
_diffrn_source_current           140
_diffrn_source_power             7.000
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    3.372
_exptl_absorpt_correction_T_max  0.8531
_exptl_absorpt_correction_T_min  0.5704
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            'yellowish orange'
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_description       plate
_exptl_crystal_F_000             2338
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.644
_refine_diff_density_min         -1.198
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1140
_refine_ls_number_reflns         17702
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0835P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1231
_refine_ls_wR_factor_ref         0.1341
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12932
_reflns_number_total             17702
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04360g2.cif
_cod_data_source_block           bs-67
_cod_depositor_comments
'Adding full bibliography for 7041874--7041876.cif.'
_cod_original_formula_sum        'C83.50 H91 B4 Cl7 F16 Fe N16 Pt2'
_cod_database_code               7041876
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H43A,H43B,H43C} of C43A, {H44A,H44B,H44C} of C44A, {H45A,
  H45B,H45C} of C45A, {H44D,H44E,H44F} of C44B, {H47A,H47B,H47C} of C47A, {H48A,
  H48B,H48C} of C48A, {H49A,H49B,H49C} of C49A, {H47D,H47E,H47F} of C47B, {H48D,
  H48E,H48F} of C48B, {H49D,H49E,H49F} of C49B, {H51A,H51B,H51C} of C51, {H52A,
  H52B,H52C} of C52, {H53A,H53B,H53C} of C53, {H80A,H80B,H80C} of C80, {H79A,
  H79B,H79C} of C79, {H78A,H78B,H78C} of C78, {H76D,H76E,H76F} of C76B, {H75D,
  H75E,H75F} of C75B, {H74D,H74E,H74F} of C74B, {H76A,H76B,H76C} of C76A, {H72D,
  H72E,H72F} of C72B, {H71D,H71E,H71F} of C71B, {H70D,H70E,H70F} of C70B, {H71A,
  H71B,H71C} of C71A, {H70A,H70B,H70C} of C70A, All C(H,H) groups
 At 1.5 times of:
  {H43D,H43E,H43F} of C43B, {H45D,H45E,H45F} of C45B, {H75A,H75B,H75C} of
  C75A, {H74A,H74B,H74C} of C74A, {H72A,H72B,H72C} of C72A
2. Restrained distances
 F9A-F10A = F9A-F11A = F9A-F12A = F10A-F11A = F10A-F12A = F11A-F12A
 2.23 with sigma of 0.05
 B4A-F13A = B4A-F14A = B4A-F15A = B4A-F16A
 1.37 with sigma of 0.03
 B4B-F13B = B4B-F14B = B4B-F15B = B4B-F16B
 1.37 with sigma of 0.03
 F13A-F14A = F13A-F15A = F13A-F16A = F14A-F15A = F14A-F16A = F15A-F16A
 2.23 with sigma of 0.05
 F13B-F14B = F13B-F15B = F13B-F16B = F14B-F15B = F14B-F16B = F15B-F16B
 2.23 with sigma of 0.05
 B3-F9A = B3-F10A = B3-F11A = B3-F12A
 1.37 with sigma of 0.01
 C43B-C45B
 2.51 with sigma of 0.02
 C43B-C42 = C45B-C42 = C44B-C42
 1.54 with sigma of 0.02
 B3-F9B = B3-F10B = B3-F11B = B3-F12B
 1.37 with sigma of 0.01
 F9B-F10B = F9B-F11B = F9B-F12B = F10B-F11B = F10B-F12B = F11B-F12B
 2.23 with sigma of 0.02
 F11B_$1-Cl4
 2.8 with sigma of 0.02
 C74A-C73 = C76A-C73 = C75A-C73
 1.54 with sigma of 0.02
 C76B-C73 = C75B-C73 = C74B-C73
 1.54 with sigma of 0.02
 C83-Cl5 = C83-Cl6
 1.76 with sigma of 0.02
 Cl5-Cl6
 2.9 with sigma of 0.02
 Cl7A-C84A
 1.76 with sigma of 0.02
 Cl8A-C84A
 1.76 with sigma of 0.02
 Cl8A-Cl7A
 2.9 with sigma of 0.02
 Cl8B-Cl7B
 2.9 with sigma of 0.02
 Cl7B-C84B = Cl8B-C84B
 1.76 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F1) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F8) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(C82) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uiso(F9A) = Uiso(F10A) = Uiso(F11A) = Uiso(F12A) = Uiso(B4A) = Uiso(F13A) =
Uiso(F14A) = Uiso(F15A) = Uiso(F16A) = Uiso(C76A) = Uiso(C75A) = Uiso(C74A)
Uiso(C75B) = Uiso(C74B) = Uiso(C76B)
Uiso(F9B) = Uiso(F10B) = Uiso(F11B) = Uiso(F12B)
Uiso(C70B) = Uiso(C72B) = Uiso(C71B)
Uiso(Cl8A) = Uiso(C84A) = Uiso(Cl7A)
Uiso(Cl6) = Uiso(C83) = Uiso(Cl5)
Uiso(Cl7B) = Uiso(C84B) = Uiso(Cl8B)
4. Others
 Fixed Sof: C43A(0.65) H43A(0.65) H43B(0.65) H43C(0.65) C44A(0.65) H44A(0.65)
 H44B(0.65) H44C(0.65) C45A(0.65) H45A(0.65) H45B(0.65) H45C(0.65) C43B(0.35)
 H43D(0.35) H43E(0.35) H43F(0.35) C44B(0.35) H44D(0.35) H44E(0.35) H44F(0.35)
 C45B(0.35) H45D(0.35) H45E(0.35) H45F(0.35) C47A(0.5) H47A(0.5) H47B(0.5)
 H47C(0.5) C48A(0.5) H48A(0.5) H48B(0.5) H48C(0.5) C49A(0.5) H49A(0.5)
 H49B(0.5) H49C(0.5) C47B(0.5) H47D(0.5) H47E(0.5) H47F(0.5) C48B(0.5)
 H48D(0.5) H48E(0.5) H48F(0.5) C49B(0.5) H49D(0.5) H49E(0.5) H49F(0.5)
 C69A(0.5) C70A(0.5) H70A(0.5) H70B(0.5) H70C(0.5) C71A(0.5) H71A(0.5)
 H71B(0.5) H71C(0.5) C72A(0.5) H72A(0.5) H72B(0.5) H72C(0.5) C69B(0.5)
 C70B(0.5) H70D(0.5) H70E(0.5) H70F(0.5) C71B(0.5) H71D(0.5) H71E(0.5)
 H71F(0.5) C72B(0.5) H72D(0.5) H72E(0.5) H72F(0.5) C74A(0.5) H74A(0.5)
 H74B(0.5) H74C(0.5) C75A(0.5) H75A(0.5) H75B(0.5) H75C(0.5) C76A(0.5)
 H76A(0.5) H76B(0.5) H76C(0.5) C74B(0.5) H74D(0.5) H74E(0.5) H74F(0.5)
 C75B(0.5) H75D(0.5) H75E(0.5) H75F(0.5) C76B(0.5) H76D(0.5) H76E(0.5)
 H76F(0.5) F9A(0.7) F10A(0.7) F11A(0.7) F12A(0.7) F9B(0.3) F10B(0.3) F11B(0.3)
 F12B(0.3) B4A(0.5) F13A(0.5) F14A(0.5) F15A(0.5) F16A(0.5) B4B(0.5) F13B(0.5)
 F14B(0.5) F15B(0.5) F16B(0.5) Cl5(0.5) Cl6(0.5) C83(0.5) H83A(0.5) H83B(0.5)
 Cl8B(0.5) Cl7B(0.5) C84B(0.5) H84A(0.5) H84B(0.5) Cl7A(0.5) C84A(0.5)
 H84C(0.5) H84D(0.5) Cl8A(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C81(H81A,H81B), C82(H82A,H82B), C83(H83A,H83B), C84B(H84A,H84B), C84A(H84C,
 H84D)
5.b Me refined with riding coordinates:
 C43B(H43D,H43E,H43F)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C7(H7), C9(H9), C10(H10), C11(H11), C14(H14),
 C15(H15), C16(H16), C18(H18), C20(H20), C22(H22), C23(H23), C24(H24), C28(H28),
  C33(H33), C35(H35), C38(H38), C40(H40), C41(H41), C54(H54), C55(H55),
 C57(H57), C60(H60), C62(H62), C65(H65), C67(H67), C68(H68)
5.d Idealised Me refined as rotating group:
 C43A(H43A,H43B,H43C), C44A(H44A,H44B,H44C), C45A(H45A,H45B,H45C), C44B(H44D,
 H44E,H44F), C45B(H45D,H45E,H45F), C47A(H47A,H47B,H47C), C48A(H48A,H48B,H48C),
 C49A(H49A,H49B,H49C), C47B(H47D,H47E,H47F), C48B(H48D,H48E,H48F), C49B(H49D,
 H49E,H49F), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C),
 C70A(H70A,H70B,H70C), C71A(H71A,H71B,H71C), C72A(H72A,H72B,H72C), C70B(H70D,
 H70E,H70F), C71B(H71D,H71E,H71F), C72B(H72D,H72E,H72F), C74A(H74A,H74B,H74C),
 C75A(H75A,H75B,H75C), C76A(H76A,H76B,H76C), C74B(H74D,H74E,H74F), C75B(H75D,
 H75E,H75F), C76B(H76D,H76E,H76F), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C),
 C80(H80A,H80B,H80C)
;
_shelx_res_checksum              18332
_olex2_submission_special_instructions 'No special instructions were received'