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_1550072
_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         'C77 H95 N7 Si2 Zn, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C77.5 H96 Cl N7 Si2 Zn'
_chemical_formula_weight         1282.61
_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     dual
_audit_creation_date             2017-02-14
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.02.06 svn.r3384 for OlexSys, GUI svn.r5312)
;
_audit_update_record
;
2017-07-27 deposited with the CCDC.
2018-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                90.736(2)
_cell_angle_beta                 91.970(2)
_cell_angle_gamma                108.933(3)
_cell_formula_units_Z            2
_cell_length_a                   13.1710(4)
_cell_length_b                   14.3764(4)
_cell_length_c                   19.9456(6)
_cell_measurement_reflns_used    19953
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5160
_cell_measurement_theta_min      2.4800
_cell_volume                     3569.14(19)
_computing_cell_refinement       'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_data_collection
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_reduction        'CrysAlisPro 1.171.39.9g (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 0.997
_diffrn_measured_fraction_theta_max 0.992
_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    -31.00  77.00   1.00   10.00    --  -13.00  72.00-120.00  108
  2  \w    -70.00  23.00   1.00   10.00    --  -13.00 -72.00 120.00   93
  3  \w    -63.00  23.00   1.00   10.00    --  -13.00 -72.00 -60.00   86
  4  \w    -85.00 -10.00   1.00   10.00    --  -13.00   0.00 120.00   75
  5  \w    -15.00   5.00   1.00   10.00    --  -13.00 -54.00 -30.00   20
  6  \w    -31.00  77.00   1.00   10.00    --  -13.00  72.00-150.00  108
  7  \w    -67.00  23.00   1.00   10.00    --  -13.00 -72.00  90.00   90
  8  \w    -65.00   7.00   1.00   10.00    --  -13.00 -72.00 -90.00   72
;
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_type
'Rigaku FRE+ equipped with VHF Varimax confocal mirrors and an AFC12 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      -0.0309726000
_diffrn_orient_matrix_UB_12      0.0247817000
_diffrn_orient_matrix_UB_13      0.0165681000
_diffrn_orient_matrix_UB_21      -0.0135431000
_diffrn_orient_matrix_UB_22      0.0167506000
_diffrn_orient_matrix_UB_23      -0.0312786000
_diffrn_orient_matrix_UB_31      -0.0458705000
_diffrn_orient_matrix_UB_32      -0.0427513000
_diffrn_orient_matrix_UB_33      -0.0037543000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0631
_diffrn_reflns_av_unetI/netI     0.0765
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            57370
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.504
_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    0.462
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67269
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.9g (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'iridescent blue-green'
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_description       plate
_exptl_crystal_F_000             1370
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.015
_refine_diff_density_max         1.161
_refine_diff_density_min         -0.904
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     897
_refine_ls_number_reflns         16242
_refine_ls_number_restraints     986
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1224
_refine_ls_R_factor_gt           0.0814
_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^)+(0.1010P)^2^+7.1998P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1989
_refine_ls_wR_factor_ref         0.2218
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11197
_reflns_number_total             16242
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc03762k2.cif
_cod_data_source_block           P1starZn
_cod_depositor_comments
'Adding full bibliography for 1550065--1550077.cif.'
_cod_original_formula_sum        'C77.50 H96 Cl N7 Si2 Zn'
_cod_database_code               1550072
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C72 H90 N6 Si2 Zn'
_reflns_odcompleteness_completeness 99.27
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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. Restrained distances
 C201-Cl22
 1.7 with sigma of 0.02
 C201-Cl21 \\sim C201-Cl22
 with sigma of 0.02
 C22-Si1 \\sim C34-Si2 \\sim C34-Si2B
 with sigma of 0.02
3. Rigid bond restraints
 C201, Cl21, Cl22
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N101, C101, C102, C103, C104, C105, N111, C111, C112, C113, C114, C115
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(Si2B) = Uanis(C35B) = Uanis(C36B) = Uanis(C37B) = Uanis(C38B) = Uanis(N6B)
Uanis(C39B) = Uanis(C40B) = Uanis(C41B)
Uanis(C42B) = Uanis(C43B) = Uanis(C44B)
Uanis(C35) = Uanis(C36) = Uanis(C37) = Uanis(C38) = Uanis(N6)
Uanis(C39) = Uanis(C40) = Uanis(C41)
Uanis(C42) = Uanis(C43) = Uanis(C44)
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
{Si2, C35, C36, C37, C38, N6, C39, C40, C41, C42, C43, C44} sigma for 1-2:
0.02, 1-3: 0.04
as
{Si2B, C35B, C36B, C37B, C38B, N6B, C39B, C40B, C41B, C42B, C43B, C44B}
{N101, C101, C102, C103, C104, C105} sigma for 1-2: 0.02, 1-3: 0.04
as
{N111, C111, C112, C113, C114, C115}
7. Others
 Sof(Si2B)=Sof(C35B)=Sof(H35C)=Sof(H35D)=Sof(C36B)=Sof(H36C)=Sof(H36D)=
 Sof(C37B)=Sof(H37C)=Sof(H37D)=Sof(C38B)=Sof(N6B)=Sof(C39B)=Sof(H39B)=Sof(C40B)=
 Sof(H40D)=Sof(H40E)=Sof(H40F)=Sof(C41B)=Sof(H41D)=Sof(H41E)=Sof(H41F)=
 Sof(C42B)=Sof(H42B)=Sof(C43B)=Sof(H43D)=Sof(H43E)=Sof(H43F)=Sof(C44B)=
 Sof(H44D)=Sof(H44E)=Sof(H44F)=1-FVAR(1)
 Sof(Si2)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C37)=
 Sof(H37A)=Sof(H37B)=Sof(C38)=Sof(N6)=Sof(C39)=Sof(H39)=Sof(C40)=Sof(H40A)=
 Sof(H40B)=Sof(H40C)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C42)=Sof(H42)=
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=
 FVAR(1)
 Sof(N111)=Sof(C111)=Sof(H111)=Sof(C112)=Sof(H112)=Sof(C113)=Sof(H113)=
 Sof(C114)=Sof(H114)=Sof(C115)=Sof(H115)=1-FVAR(2)
 Sof(N101)=Sof(C101)=Sof(H101)=Sof(C102)=Sof(H102)=Sof(C103)=Sof(H103)=
 Sof(C104)=Sof(H104)=Sof(C105)=Sof(H105)=FVAR(2)
 Fixed Sof: Cl22(0.5) C201(0.5) H20A(0.5) H20B(0.5) Cl21(0.5)
8.a Ternary CH refined with riding coordinates:
 C30(H30), C27(H27), C39(H39), C42(H42), C39B(H39B), C42B(H42B)
8.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C35(H35A,H35B), C36(H36A,
 H36B), C37(H37A,H37B), C201(H20A,H20B), C35B(H35C,H35D), C36B(H36C,H36D),
 C37B(H37C,H37D)
8.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C7(H7), C8(H8), C12(H12), C13(H13), C17(H17), C18(H18),
 C46(H46), C48(H48), C50(H50), C60(H60), C62(H62), C64(H64), C101(H101),
 C102(H102), C103(H103), C104(H104), C105(H105), C111(H111), C112(H112),
 C113(H113), C114(H114), C115(H115)
8.d Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C44(H44A,
 H44B,H44C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C),
 C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C66(H66A,H66B,
 H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C70(H70A,H70B,H70C), C71(H71A,
 H71B,H71C), C72(H72A,H72B,H72C), C40B(H40D,H40E,H40F), C41B(H41D,H41E,H41F),
 C43B(H43D,H43E,H43F), C44B(H44D,H44E,H44F)
;
_shelx_res_checksum              6210
_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 1.501
_oxdiff_exptl_absorpt_empirical_full_min 0.584