K⊂{[FeII(Tp)(CN)3]4[CoIII(pzTp)]3[CoII(pzTp)]}: a neutral soluble model complex of photomagnetic Prussian blue analogues
Garnier, D.; Jiménez, J.-R.; Li, Y.; von Bardeleben, J.; Journaux, Y.; Augenstein, T.; Moos, E. M. B.; Gamer, M. T.; Breher, F.; Lescouëzec, R.; Chem. Sci. 7 (2016) 4825–; doi:10.1039/C6SC01435F

data_1543323
_publ_section_title
;
 K&#x2282;{[FeII(Tp)(CN)3]4[CoIII(pzTp)]3[CoII(pzTp)]}: a neutral soluble
 model complex of photomagnetic Prussian blue analogues
;
_journal_issue                   8
_journal_name_full               'Chem. Sci.'
_journal_page_first              4825
_journal_paper_doi               10.1039/C6SC01435F
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C96 H88 B8 Co4 Fe4 K1 N68'
_chemical_formula_sum            'C96 H88 B8 Co4 Fe4 K N68'
_chemical_formula_weight         2779.04
_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
_audit_creation_date             2016-03-18
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-03-18 deposited with the CCDC.
2016-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                84.336(2)
_cell_angle_beta                 81.254(2)
_cell_angle_gamma                71.749(2)
_cell_formula_units_Z            2
_cell_length_a                   16.4051(5)
_cell_length_b                   17.4587(5)
_cell_length_c                   29.8313(8)
_cell_measurement_reflns_used    36514
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.21
_cell_measurement_theta_min      1.32
_cell_volume                     8008.0(4)
_computing_cell_refinement       'STOE X-AREA, PLATON (A.L.Spek, 2009)'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED & LANA, PLATON (A.L.Spek, 2009)'
_computing_molecular_graphics
'Diamond 2/3/4, Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'MS Word, Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2014/7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CMOS pixel detector'
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'Dectris Pilatus 100k'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'single reflection optic'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0658
_diffrn_reflns_av_unetI/netI     0.0912
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            67140
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.185
_diffrn_reflns_theta_min         1.318
_diffrn_source                   'Mo LFF Sealed Tube'
_diffrn_source_type              'Xenocs Genix3D microfocus'
_exptl_absorpt_coefficient_mu    0.839
_exptl_absorpt_correction_T_max  0.9980
_exptl_absorpt_correction_T_min  0.9915
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED, X-SHAPE & LANA'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_description       plate
_exptl_crystal_F_000             2822
_exptl_crystal_size_max          0.433
_exptl_crystal_size_mid          0.309
_exptl_crystal_size_min          0.142
_refine_diff_density_max         0.943
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.860
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1873
_refine_ls_number_reflns         31472
_refine_ls_number_restraints     279
_refine_ls_restrained_S_all      0.861
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0527
_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^)+(0.0519P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1243
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18783
_reflns_number_total             31472
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc01435f2.cif
_cod_data_source_block           dg464_sq
_cod_depositor_comments          'Adding full bibliography for 1543323.cif.'
_cod_database_code               1543323
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All B(H,H) groups, All C(H) groups
2. Uiso/Uaniso restraints and constraints
B6A \\sim B6B: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
N630 \\sim N680: within 1.7A with sigma of 0.004 and sigma for terminal atoms
of 0.008
N221 \\sim N271: within 1.7A with sigma of 0.004 and sigma for terminal atoms
of 0.008
N530 \\sim N580: within 1.7A with sigma of 0.008 and sigma for terminal atoms
of 0.016
N680 \\sim N681 \\sim C680 \\sim C681 \\sim C682: within 1.7A with sigma of
0.004 and sigma for terminal atoms of 0.008
C730 \\sim N730 \\sim N731 \\sim C732 \\sim C731: within 1.7A with sigma of
0.004 and sigma for terminal atoms of 0.008
N780 \\sim N781 \\sim C780 \\sim C781 \\sim C782 \\sim B7: within 2A with sigma
of 0.008 and sigma for terminal atoms of 0.016
3. Rigid body (RIGU) restrains
 N650, N651, C650, C651, C652, B6B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N580, N581, C580, C581, C582
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N270, N271, C270, C271, C272
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N220, N221, C220, C221, C222
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N630, N631, C630, C631, C632
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Fixed Sof: K1A(0.5) K1B(0.2) K1C(0.2) K1D(0.1) N220(0.66667) N221(0.66667)
 N530(0.6) N531(0.6) N600(0.66667) N601(0.66667) N630(0.66667) N631(0.66667)
 N730(0.7) N731(0.7) N271(0.33333) C272(0.33333) H272(0.33333) C271(0.33333)
 H271(0.33333) C270(0.33333) H270(0.33333) N270(0.33333) N580(0.4) N581(0.4)
 N650(0.33333) N651(0.33333) N680(0.33333) N681(0.33333) C682(0.33333)
 H682(0.33333) C681(0.33333) H681(0.33333) C680(0.33333) H680(0.33333)
 N780(0.3) N781(0.3) C220(0.66667) H220(0.66667) C221(0.66667) H221(0.66667)
 C222(0.66667) H222(0.66667) C530(0.6) H530(0.6) C531(0.6) H531(0.6) C532(0.6)
 H532(0.6) C600(0.66667) H600(0.66667) C601(0.66667) H601(0.66667)
 C602(0.66667) H602(0.66667) C630(0.66667) H630(0.66667) C631(0.66667)
 H631(0.66667) C632(0.66667) H632(0.66667) C730(0.7) H730(0.7) C731(0.7)
 H731(0.7) C732(0.7) H732(0.7) C580(0.4) H580(0.4) C581(0.4) H581(0.4)
 C582(0.4) H582(0.4) C650(0.33333) H650(0.33333) C651(0.33333) H651(0.33333)
 C652(0.33333) H652(0.33333) C780(0.3) H780(0.3) C781(0.3) H781(0.3) C782(0.3)
 H782(0.3) H2A(0.66667) H2B(0.33333) B6A(0.66667) B6B(0.33333)
5.a Ternary CH refined with riding coordinates:
 B1(H1), B2(H2A), B2(H2B), B3(H3), B4(H4)
5.b Aromatic/amide H refined with riding coordinates:
 C830(H830), C272(H272), C271(H271), C270(H270), C682(H682), C681(H681),
 C680(H680), C1T(H1T), C100(H100), C101(H101), C102(H102), C110(H110),
 C111(H111), C112(H112), C120(H120), C121(H121), C122(H122), C200(H200),
 C201(H201), C202(H202), C210(H210), C211(H211), C212(H212), C300(H300),
 C301(H301), C302(H302), C310(H310), C312(H312), C320(H320), C321(H321),
 C322(H322), C400(H400), C401(H401), C402(H402), C410(H410), C411(H411),
 C412(H412), C420(H420), C421(H421), C422(H422), C500(H500), C501(H501),
 C502(H502), C510(H510), C511(H511), C512(H512), C520(H520), C521(H521),
 C522(H522), C610(H610), C611(H611), C612(H612), C620(H620), C621(H621),
 C622(H622), C700(H700), C701(H701), C702(H702), C710(H710), C711(H711),
 C712(H712), C720(H720), C721(H721), C722(H722), C800(H800), C801(H801),
 C802(H802), C810(H810), C811(H811), C812(H812), C820(H820), C821(H821),
 C822(H822), C832(H832), C831(H831), C220(H220), C221(H221), C222(H222),
 C530(H530), C531(H531), C532(H532), C600(H600), C601(H601), C602(H602),
 C630(H630), C631(H631), C632(H632), C730(H730), C731(H731), C732(H732),
 C580(H580), C581(H581), C582(H582), C650(H650), C651(H651), C652(H652),
 C780(H780), C781(H781), C782(H782)
5.c Fitted pentagon refined as free rotating group:
 N271(C272,C271,C270,N270), N680(N681,C682,C681,C680)
;
_shelx_res_checksum              93505
_shelx_fab_checksum              27403
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'