Phthalocyanine-polyoxotungstate lanthanide double deckers.
Sarwar, Sidra; Sanz, Sergio; van Leusen, Jan; Nichol, Gary S.; Brechin, Euan K.; Kögerler, Paul; Dalton transactions (Cambridge, England : 2003) 49 (2020) 16638–16642; doi:10.1039/d0dt03716h

data_7705845
_publ_section_title
;
 Phthalocyanine-polyoxotungstate lanthanide double deckers.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16638
_journal_page_last               16642
_journal_paper_doi               10.1039/d0dt03716h
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety
'C32 H18 N8 O39 P Tb W11, 2(C16 H36 N), 2(C6 H16 N), 6[CH2Cl2]'
_chemical_formula_sum            'C82 H134 Cl12 N12 O39 P Tb W11'
_chemical_formula_weight         4549.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-24
_audit_creation_method
;
Olex2 1.3-beta
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-03-27 deposited with the CCDC.	2020-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.3550(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.5917(14)
_cell_length_b                   21.7413(12)
_cell_length_c                   26.2648(15)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      20.256
_cell_measurement_theta_min      2.206
_cell_volume                     12844.3(13)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_type            PILATUS_2M_S_N_24_0107_Diamond
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0833
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            53920
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        20.294
_diffrn_reflns_theta_max         20.294
_diffrn_reflns_theta_min         1.263
_diffrn_source                   Synchrotron
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.767
_exptl_absorpt_correction_T_max  0.4252
_exptl_absorpt_correction_T_min  0.2214
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1335 before and 0.0955 after correction.
The Ratio of minimum to maximum transmission is 0.5207.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.353
_exptl_crystal_description       plate
_exptl_crystal_F_000             8480
_exptl_crystal_recrystallization_method
'The material was recrystallised from dichloromethane by slow evaporation'
_exptl_crystal_size_max          0.048
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.798
_refine_diff_density_min         -0.814
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         7102
_refine_ls_number_restraints     931
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0509
_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^)+(0.0801P)^2^+77.3435P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1470
_refine_ls_wR_factor_ref         0.1507
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5609
_reflns_number_total             7102
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03716h2.cif
_cod_data_source_block           eb20034
_cod_database_code               7705845
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.829
_shelx_estimated_absorpt_t_min   0.651
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H25a,H25b,H25c,H25d,H25e,H25f} of C25, {H33a,H33b,H33c,
  H33d,H33e,H33f} of C33, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, {H39d,H39e,H39f,H39a,H39b,H39c} of C39, {H41d,H41e,
  H41f,H41a,H41b,H41c} of C41
2. Restrained distances
 N6-C26 = N6-C22 = N6-C18 = N6-C30 = C26-C27 = C22-C23 = C18-C19 = C30-C31 =
 C27-C28
 1.52 with sigma of 0.02
 C23-C24 = C19-C20 = C31-C32
 1.53 with sigma of 0.02
 C28-C29 = C24-C25 = C20-C21 = C32-C33
 1.49 with sigma of 0.02
 C39-C38 = N8-C38 = N8-C40A = C41-C40A = C35-C34 = N7-C34 = N7-C36 = C37-C36
 1.49 with sigma of 0.02
 N8-H8
 0.84 with sigma of 0.02
 N6-C23 = N6-C31
 2.59 with sigma of 0.04
 C27-C29 = C23-C25 = C19-C21 = C31-C33
 2.53 with sigma of 0.04
 N6-C27 = N6-C19
 2.56 with sigma of 0.04
 C26-C28 = C22-C24 = C18-C20 = C30-C32
 2.48 with sigma of 0.04
 C39-N8
 2.5 with sigma of 0.04
 C41-N8
 2.5 with sigma of 0.04
 C37-N7
 2.5 with sigma of 0.04
 C35-N7
 2.5 with sigma of 0.04
 N6-C26 \\sim N6-C22 \\sim N6-C18 \\sim N6-C30
 with sigma of 0.02
 C26-C27 \\sim C27-C28 \\sim C28-C29 \\sim C30-C31 \\sim C31-C32 \\sim C32-C33
\\sim C18-C19 \\sim C19-C20
 \\sim C20-C21 \\sim C22-C23 \\sim C23-C24 \\sim C24-C25
 with sigma of 0.02
 C26-C28 \\sim C27-C29 \\sim C30-C32 \\sim C31-C33 \\sim C18-C20 \\sim C19-C21
\\sim C22-C24 \\sim C23-C25
 with sigma of 0.04
 C26-C30 \\sim C30-C18 \\sim C18-C22
 with sigma of 0.04
 C10_$1-C10 \\sim C2-C9
 with sigma of 0.02
 C13-C13_$1 \\sim C6-C5
 with sigma of 0.02
 C13-C12 \\sim C7-C6
 with sigma of 0.02
 C11-C10 \\sim C9-C8
 with sigma of 0.02
 C11-C11_$1 \\sim C8-C3
 with sigma of 0.02
 N3-C10 \\sim N1-C9
 with sigma of 0.02
 C12-C11 \\sim C8-C7
 with sigma of 0.02
 C17-C17_$1 \\sim C6-C5
 with sigma of 0.02
 C14-C14_$1 \\sim C2-C9
 with sigma of 0.02
 C16-C15 \\sim C8-C7
 with sigma of 0.02
 C17-C16 \\sim C7-C6
 with sigma of 0.02
 N5-C14 \\sim N1-C9
 with sigma of 0.02
 C15-C14 \\sim C9-C8
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N6 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim
C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim
C33: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
4. 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
5. Others
 1*[Sof(C39)]+1*[Sof(C41)]=1.5 with esd of 0.001
 1*[Sof(C38)]+1*[Sof(C38A)]=0.75 with esd of 0.001
 1*[Sof(C40)]+1*[Sof(C40A)]=0.75 with esd of 0.001
 Fixed Sof: H25a(0.5) H25b(0.5) H25c(0.5) H25d(0.5) H25e(0.5) H25f(0.5)
 H33a(0.5) H33b(0.5) H33c(0.5) H33d(0.5) H33e(0.5) H33f(0.5) H36a(0.5)
 H36b(0.5) H37b(0.5) H37c(0.5) H38a(0.25) H38b(0.25) H38c(0.25) H38d(0.25)
 H39d(0.25) H39e(0.5) H39f(0.5) H39a(0.5) H39b(0.5) H39c(0.5) H40a(0.25)
 H40b(0.25) H40c(0.25) H40d(0.25) H41d(0.5) H41e(0.5) H41f(0.25) H41a(0.5)
 H41b(0.5) H41c(0.5) H8(0.5)
6.a Everything fixed:
 N7, C34, C35, C36, C37, N8, C38, C38A, C39, C40, C40A, C41
6.b Ternary CH refined with riding coordinates:
 N7(H7a)
6.c Secondary CH2 refined with riding coordinates:
 C18(H18a,H18b), C19(H19a,H19b), C20(H20a,H20b), C22(H22a,H22b), C23(H23a,
 H23b), C24(H24a,H24b), C26(H26a,H26b), C27(H27a,H27b), C28(H28a,H28b),
 C30(H30a,H30b), C31(H31a,H31b), C32(H32a,H32b), C34(H34a,H34b), C36(H36a,H36b),
  C38(H38a,H38b), C38A(H38c,H38d), C40(H40a,H40b), C40A(H40c,H40d)
6.d Me refined with riding coordinates:
 C35(H35a,H35b,H35c), C37(H37a,H37b,H37c), C39(H39d,H39e,H39f), C39(H39a,H39b,
 H39c), C41(H41d,H41e,H41f), C41(H41a,H41b,H41c)
6.e Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C12(H12), C13(H13), C16(H16), C17(H17)
6.f Fitted hexagon refined as free rotating group:
 C3(C4,C5,C6,C7,C8)
6.g Disordered Me refined with riding coordinates:
 C25(H25a,H25b,H25c,H25d,H25e,H25f), C33(H33a,H33b,H33c,H33d,H33e,H33f)
6.h Idealised Me refined as rotating group:
 C21(H21a,H21b,H21c), C29(H29a,H29b,H29c)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              52546
_shelx_fab_checksum              93457
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 800'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone oil.'
_olex2_submission_original_sample_id SS-358
_olex2_submission_special_instructions 'No special instructions were received'