Variable coordination of carbazolyl-bis(tetrazole) ligands in lanthanide chemistry.
Gajecki, Leah; Berg, David J.; Hoenisch, Josh; Oliver, Allen G.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 15487–15496; doi:10.1039/c8dt02757a

data_7047758
_publ_section_title
;
 Variable coordination of carbazolyl-bis(tetrazole) ligands in lanthanide
 chemistry.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15487
_journal_page_last               15496
_journal_paper_doi               10.1039/c8dt02757a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C59 H80 N18 O Si Yb'
_chemical_formula_sum            'C75.31 H99.64 N18 O Si Yb'
_chemical_formula_weight         1474.21
_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             2018-09-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-27 deposited with the CCDC.
2018-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                82.905(3)
_cell_angle_beta                 88.389(3)
_cell_angle_gamma                87.902(3)
_cell_formula_units_Z            2
_cell_length_a                   13.0237(13)
_cell_length_b                   15.8464(15)
_cell_length_c                   18.8408(19)
_cell_measurement_reflns_used    9792
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.04
_cell_measurement_theta_min      2.37
_cell_volume                     3854.9(7)
_computing_cell_refinement       'Bruker SAINT (Bruker, 2015)'
_computing_data_collection       'Bruker APEX-3 (Bruker, 2015)'
_computing_data_reduction        'Bruker SAINT (Bruker, 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      150.15
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker PHOTON-100 CMOS'
_diffrn_measurement_method       'combination of \w and \f-scans '
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0730
_diffrn_reflns_av_unetI/netI     0.0667
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            59476
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         29.224
_diffrn_reflns_theta_min         1.954
_diffrn_source                   synchrotorn
_exptl_absorpt_coefficient_mu    1.580
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.5794
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Krause et al., 2015)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_description       rod
_exptl_crystal_F_000             1539
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.222
_refine_diff_density_min         -1.079
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     832
_refine_ls_number_reflns         15886
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0411P)^2^+11.9245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1263
_refine_ls_wR_factor_ref         0.1417
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12359
_reflns_number_total             15886
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02757a2.cif
_cod_data_source_block           Compound_4a_sq
_cod_depositor_comments
'Adding full bibliography for 7047755--7047762.cif.'
_cod_database_code               7047758
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.845
_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
 C17-C18 \\sim C17-C19 \\sim C17-C20 \\sim C17-C18A \\sim C17-C19A \\sim
C17-C20A
 with sigma of 0.01
 C41-C42 \\sim C41-C43 \\sim C41-C44 \\sim C41-C42A \\sim C41-C43A \\sim
C41-C44A
 with sigma of 0.01
 C50-C51 \\sim C50-C52 \\sim C50-C51A \\sim C50-C52A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C18 \\sim C18A \\sim C19 \\sim C19A \\sim C20 \\sim C20A: within 2A with sigma
of 0.005 and sigma for terminal atoms of 0.01
C23 \\sim C23A \\sim C24 \\sim C24A: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
C42 \\sim C42A \\sim C43 \\sim C43A \\sim C44 \\sim C44A: within 2A with sigma
of 0.005 and sigma for terminal atoms of 0.01
C51 \\sim C51A \\sim C52 \\sim C52A: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
4. Others
 Fixed Sof: C18(0.5) H18A(0.5) H18B(0.5) H18C(0.5) C19(0.5) H19A(0.5)
 H19B(0.5) C20(0.5) H20A(0.5) H20B(0.5) C18A(0.5) H18D(0.5) H18E(0.5) H18F(0.5)
 C19A(0.5) H19C(0.5) H19D(0.5) H19E(0.5) C20A(0.5) H20C(0.5) H20D(0.5)
 H20E(0.5) H22(0.66667) H22A(0.33333) C23(0.66667) H23A(0.66667) H23B(0.66667)
 H23C(0.66667) C24(0.66667) H24A(0.66667) H24B(0.66667) H24C(0.66667)
 C23A(0.33333) H23D(0.33333) H23E(0.33333) H23F(0.33333) C24A(0.33333)
 H24D(0.33333) H24E(0.33333) H24F(0.33333) C42(0.5) H42A(0.5) H42B(0.5)
 H42C(0.5) C43(0.5) H43A(0.5) H43B(0.5) H43C(0.5) C44(0.5) H44A(0.5) H44B(0.5)
 H44C(0.5) C42A(0.5) H42D(0.5) H42E(0.5) H42F(0.5) C43A(0.5) H43D(0.5)
 H43E(0.5) H43F(0.5) C44A(0.5) H44D(0.5) H44E(0.5) H44F(0.5) H50(0.5) H50A(0.5)
 C51(0.5) H51A(0.5) H51B(0.5) H51C(0.5) C52(0.5) H52A(0.5) H52B(0.5) H52C(0.5)
 C51A(0.5) H51D(0.5) H51E(0.5) H51F(0.5) C52A(0.5) H52D(0.5) H52E(0.5) H52F(0.5)
5.a Ternary CH refined with riding coordinates:
 C22(H22), C22(H22A), C26(H26), C50(H50), C50(H50A), C54(H54)
5.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C20(H20A,H20B)
5.c Me refined with riding coordinates:
 C18(H18A,H18B,H18C), C18A(H18D,H18E,H18F), C19A(H19C,H19D,H19E), C20A(H20C,
 H20D,H20E), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C),
 C42A(H42D,H42E,H42F), C43A(H43D,H43E,H43F), C44A(H44D,H44E,H44F)
5.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C10(H10), C31(H31), C33(H33), C36(H36), C38(H38)
5.e Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C23A(H23D,H23E,H23F), C24A(H24D,H24E,H24F),
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C46(H46A,H46B,H46C), C47(H47A,H47B,
 H47C), C48(H48A,H48B,H48C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C),
 C51A(H51D,H51E,H51F), C52A(H52D,H52E,H52F), C55(H55A,H55B,H55C), C56(H56A,H56B,
 H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C)
;
_shelx_res_checksum              11237
_shelx_fab_checksum              43958
_olex2_submission_special_instructions 'No special instructions were received'