Tailored homo- and hetero- lanthanide porphyrin dimers: a synthetic strategy for integrating multiple spintronic functionalities into a single molecule.
Le Roy, Jennifer J.; Cremers, Jonathan; Thomlinson, Isabel A.; Slota, Michael; Myers, William K.; Horton, Peter H.; Coles, Simon J.; Anderson, Harry L.; Bogani, Lapo; Chemical science 9 (2018) 8474–8481; doi:10.1039/c8sc03762k

data_1550071
_publ_section_title
;
 Tailored homo- and hetero- lanthanide porphyrin dimers: a synthetic
 strategy for integrating multiple spintronic functionalities into a
 single molecule.
;
_journal_issue                   45
_journal_name_full               'Chemical science'
_journal_page_first              8474
_journal_page_last               8481
_journal_paper_doi               10.1039/c8sc03762k
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         '1(C78 H107 Co Dy N4 O9 P3 Si)'
_chemical_formula_sum            'C78 H107 Co Dy N4 O9 P3 Si'
_chemical_formula_weight         1587.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-09-08
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_audit_update_record
;
2017-07-27 deposited with the CCDC.
2018-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.4603(9)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.34446(16)
_cell_length_b                   39.8242(4)
_cell_length_c                   20.5371(2)
_cell_measurement_reflns_used    69644
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5390
_cell_measurement_theta_min      1.7780
_cell_volume                     15820.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -104.00   2.00   0.50   30.00    --  -22.00 -72.00  30.00  212
  2  \w    -66.00  31.00   0.50   30.00    --  -22.00  72.00-180.00  194
  3  \w   -100.00 -14.00   0.50   30.00    --  -22.00  18.00-180.00  172
  4  \w    -87.00  68.00   0.50   30.00    --  -22.00   0.00  30.00  310
  5  \w   -100.00   9.00   0.50   30.00    --  -22.00 -72.00  60.00  218
;
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_type
'Rigaku FRE+ equipped with HF Varimax confocal mirrors and an AFC10 goniometer and HG Saturn 724+ detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0086486000
_diffrn_orient_matrix_UB_12      -0.0120809000
_diffrn_orient_matrix_UB_13      -0.0241610000
_diffrn_orient_matrix_UB_21      0.0320759000
_diffrn_orient_matrix_UB_22      0.0029100000
_diffrn_orient_matrix_UB_23      -0.0154969000
_diffrn_orient_matrix_UB_31      0.0154839000
_diffrn_orient_matrix_UB_32      -0.0127630000
_diffrn_orient_matrix_UB_33      0.0192271000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            163836
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         1.468
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    1.279
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81540
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'iridescent blue'
_exptl_crystal_colour_modifier   iridescent
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       'Cut Blade'
_exptl_crystal_F_000             6616
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.035
_refine_diff_density_max         2.199
_refine_diff_density_min         -0.956
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2201
_refine_ls_number_reflns         36158
_refine_ls_number_restraints     2414
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0588
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+55.1090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1289
_refine_ls_wR_factor_ref         0.1387
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27568
_reflns_number_total             36158
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc03762k2.cif
_cod_data_source_block           P1dashDy
_cod_depositor_comments
'Adding full bibliography for 1550065--1550077.cif.'
_cod_database_code               1550071
_chemical_oxdiff_formula         'C78 H107 Co Dy N4 O9 P3 Si'
_reflns_odcompleteness_completeness 99.61
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9615(5) 0.0385(5)
2. 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
3. Restrained distances
 Si1-C29 \\sim Si1-C29A
 with sigma of 0.02
 C48-C52 \\sim C48-C52A
 with sigma of 0.02
 Si81-C106 \\sim Si81-C206
 with sigma of 0.02
 C128-C132 \\sim C128-C232
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O89) = Uanis(O84B)
Uanis(O86) = Uanis(O87B)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{Co2, P81, P82, P83, O81, O82, O83, O84, O85, O86, O87, O88, O89, C142, C143,
C144, C145, C146, C147, C148, C149, C150, C151, C152, C153} sigma for 1-2:
0.02, 1-3: 0.04
as
{Co3, P81B, P82B, P83B, O81B, O82B, O83B, O84B, O85B, O86B, O87B, O88B, O89B,
C242, C243, C244, C245, C246, C247, C248, C249, C250, C251, C252, C253}
{C154, C155, C156, C157, C158} sigma for 1-2: 0.01, 1-3: 0.04
as
{C254, C255, C256, C257, C258}
{C29, C30, C31} sigma for 1-2: 0.02, 1-3: 0.04
as
{C29A, C30A, C31A}
{C52, C53, C54, C55} sigma for 1-2: 0.02, 1-3: 0.04
as
{C52A, C53A, C54A, C55A}
{C132, C133, C134, C135} sigma for 1-2: 0.02, 1-3: 0.04
as
{C232, C233, C234, C235}
{C106, C107, C108} sigma for 1-2: 0.02, 1-3: 0.04
as
{C206, C207, C208}
7. Others
 Sof(Co3)=Sof(P81B)=Sof(P82B)=Sof(P83B)=Sof(O81B)=Sof(O82B)=Sof(O83B)=
 Sof(O84B)=Sof(O85B)=Sof(O86B)=Sof(O87B)=Sof(O88B)=Sof(O89B)=Sof(C242)=
 Sof(H24A)=Sof(H24B)=Sof(C243)=Sof(H24C)=Sof(H24D)=Sof(H24E)=Sof(C244)=
 Sof(H24F)=Sof(H24G)=Sof(C245)=Sof(H24H)=Sof(H24I)=Sof(H24J)=Sof(C246)=
 Sof(H24K)=Sof(H24L)=Sof(C247)=Sof(H24M)=Sof(H24N)=Sof(H24O)=Sof(C248)=
 Sof(H24P)=Sof(H24Q)=Sof(C249)=Sof(H24R)=Sof(H24S)=Sof(H24T)=Sof(C250)=
 Sof(H25A)=Sof(H25B)=Sof(C251)=Sof(H25C)=Sof(H25D)=Sof(H25E)=Sof(C252)=
 Sof(H25F)=Sof(H25G)=Sof(C253)=Sof(H25H)=Sof(H25I)=Sof(H25J)=Sof(C254)=
 Sof(H254)=Sof(C255)=Sof(H255)=Sof(C256)=Sof(H256)=Sof(C257)=Sof(H257)=
 Sof(C258)=Sof(H258)=1-FVAR(1)
 Sof(Co2)=Sof(P81)=Sof(P82)=Sof(P83)=Sof(O81)=Sof(O82)=Sof(O83)=Sof(O84)=
 Sof(O85)=Sof(O86)=Sof(O87)=Sof(O88)=Sof(O89)=Sof(C142)=Sof(H14A)=Sof(H14B)=
 Sof(C143)=Sof(H14C)=Sof(H14D)=Sof(H14E)=Sof(C144)=Sof(H14F)=Sof(H14G)=
 Sof(C145)=Sof(H14H)=Sof(H14I)=Sof(H14J)=Sof(C146)=Sof(H14K)=Sof(H14L)=
 Sof(C147)=Sof(H14M)=Sof(H14N)=Sof(H14O)=Sof(C148)=Sof(H14P)=Sof(H14Q)=
 Sof(C149)=Sof(H14R)=Sof(H14S)=Sof(H14T)=Sof(C150)=Sof(H15A)=Sof(H15B)=
 Sof(C151)=Sof(H15C)=Sof(H15D)=Sof(H15E)=Sof(C152)=Sof(H15F)=Sof(H15G)=
 Sof(C153)=Sof(H15H)=Sof(H15I)=Sof(H15J)=Sof(C154)=Sof(H154)=Sof(C155)=
 Sof(H155)=Sof(C156)=Sof(H156)=Sof(C157)=Sof(H157)=Sof(C158)=Sof(H158)=FVAR(1)
 Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C31A)=
 Sof(H31D)=Sof(H31E)=Sof(H31F)=1-FVAR(2)
 Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C31)=Sof(H31A)=
 Sof(H31B)=Sof(H31C)=FVAR(2)
 Sof(C52A)=Sof(C53A)=Sof(H53D)=Sof(H53E)=Sof(H53F)=Sof(C54A)=Sof(H54D)=
 Sof(H54E)=Sof(H54F)=Sof(C55A)=Sof(H55D)=Sof(H55E)=Sof(H55F)=1-FVAR(3)
 Sof(C52)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=Sof(C54)=Sof(H54A)=Sof(H54B)=
 Sof(H54C)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H55C)=FVAR(3)
 Sof(C232)=Sof(C233)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C234)=Sof(H23D)=
 Sof(H23E)=Sof(H23F)=Sof(C235)=Sof(H23G)=Sof(H23H)=Sof(H23I)=1-FVAR(4)
 Sof(C132)=Sof(C133)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C134)=Sof(H13D)=
 Sof(H13E)=Sof(H13F)=Sof(C135)=Sof(H13G)=Sof(H13H)=Sof(H13I)=FVAR(4)
 Sof(C206)=Sof(H206)=Sof(C207)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C208)=
 Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(5)
 Sof(C106)=Sof(H106)=Sof(C107)=Sof(H10G)=Sof(H10H)=Sof(H10I)=Sof(C108)=
 Sof(H10J)=Sof(H10K)=Sof(H10L)=FVAR(5)
8.a Ternary CH refined with riding coordinates:
 C103(H103), C106(H106), C109(H109), C23(H23), C26(H26), C29(H29), C29A(H29A),
 C206(H206)
8.b Secondary CH2 refined with riding coordinates:
 C142(H14A,H14B), C144(H14F,H14G), C146(H14K,H14L), C148(H14P,H14Q), C150(H15A,
 H15B), C152(H15F,H15G), C242(H24A,H24B), C244(H24F,H24G), C246(H24K,H24L),
 C248(H24P,H24Q), C250(H25A,H25B), C252(H25F,H25G), C62(H62A,H62B), C64(H64A,
 H64B), C66(H66A,H66B), C68(H68A,H68B), C70(H70A,H70B), C72(H72A,H72B)
8.c Aromatic/amide H refined with riding coordinates:
 C154(H154), C155(H155), C156(H156), C157(H157), C158(H158), C82(H82),
 C83(H83), C87(H87), C88(H88), C92(H92), C93(H93), C97(H97), C98(H98),
 C113(H113), C115(H115), C117(H117), C127(H127), C129(H129), C131(H131),
 C254(H254), C255(H255), C256(H256), C257(H257), C258(H258), C2(H2), C3(H3),
 C7(H7), C8(H8), C12(H12), C13(H13), C17(H17), C18(H18), C33(H33), C35(H35),
 C37(H37), C47(H47), C49(H49), C51(H51), C74(H74), C75(H75), C76(H76), C77(H77),
  C78(H78)
8.d Idealised Me refined as rotating group:
 C143(H14C,H14D,H14E), C145(H14H,H14I,H14J), C147(H14M,H14N,H14O), C149(H14R,
 H14S,H14T), C151(H15C,H15D,H15E), C153(H15H,H15I,H15J), C104(H10A,H10B,H10C),
 C105(H10D,H10E,H10F), C107(H10G,H10H,H10I), C108(H10J,H10K,H10L), C110(H11A,
 H11B,H11C), C111(H11D,H11E,H11F), C119(H11G,H11H,H11I), C120(H12A,H12B,H12C),
 C121(H12D,H12E,H12F), C123(H12G,H12H,H12I), C124(H12J,H12K,H12L), C125(H12M,
 H12N,H12O), C133(H13A,H13B,H13C), C134(H13D,H13E,H13F), C135(H13G,H13H,H13I),
 C137(H13J,H13K,H13L), C138(H13M,H13N,H13O), C139(H13P,H13Q,H13R), C243(H24C,
 H24D,H24E), C245(H24H,H24I,H24J), C247(H24M,H24N,H24O), C249(H24R,H24S,H24T),
 C251(H25C,H25D,H25E), C253(H25H,H25I,H25J), C24(H24U,H24V,H24W), C25(H25K,H25L,
 H25M), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,
 H31B,H31C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C),
 C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C53(H53A,H53B,
 H53C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C57(H57A,H57B,H57C), C58(H58A,
 H58B,H58C), C59(H59A,H59B,H59C), C63(H63A,H63B,H63C), C65(H65A,H65B,H65C),
 C67(H67A,H67B,H67C), C69(H69A,H69B,H69C), C71(H71A,H71B,H71C), C73(H73A,H73B,
 H73C), C30A(H30D,H30E,H30F), C31A(H31D,H31E,H31F), C53A(H53D,H53E,H53F),
 C54A(H54D,H54E,H54F), C55A(H55D,H55E,H55F), C233(H23A,H23B,H23C), C234(H23D,
 H23E,H23F), C235(H23G,H23H,H23I), C207(H20A,H20B,H20C), C208(H20D,H20E,H20F)
8.e :
 C141(H141), C61(H61)
;
_shelx_res_checksum              40099
_shelx_shelxl_version_number     2014/7
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.483
_oxdiff_exptl_absorpt_empirical_full_min 0.755