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_7047762
_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         'C62 H90 Ce N19 Si2, 2.5(C7 H8)'
_chemical_formula_sum            'C79.5 H110 Ce N19 Si2'
_chemical_formula_weight         1528.16
_chemical_melting_point          563
_chemical_name_common            Ce(CzTiPr)2[N(SiMe3)2]
_chemical_name_systematic
'Bis(1,8-Bis(2?-H-tetrazo-5?-yl)-3,6-di-tert-butylcarbazolyl)(bis(trimethylsilyl)amido) cerium(III)'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-11-04
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2018-07-04 deposited with the CCDC.
2018-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 128.185(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   40.053(7)
_cell_length_b                   18.203(3)
_cell_length_c                   28.621(5)
_cell_measurement_reflns_used    9688
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.587
_cell_measurement_theta_min      2.240
_cell_volume                     16402(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (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      119.9
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            175948
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.105
_diffrn_reflns_theta_min         1.793
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.638
_exptl_absorpt_correction_T_max  0.9651
_exptl_absorpt_correction_T_min  0.8649
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0546 before and 0.0505 after correction.
The Ratio of minimum to maximum transmission is 0.8962.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_description       block
_exptl_crystal_F_000             6448
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene'
_exptl_crystal_size_max          0.305
_exptl_crystal_size_mid          0.221
_exptl_crystal_size_min          0.167
_refine_diff_density_max         1.412
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.079
_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     1026
_refine_ls_number_reflns         18106
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0372P)^2^+61.0903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.1013
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15130
_reflns_number_total             18106
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02757a2.cif
_cod_data_source_block           lg0323
_cod_depositor_comments
'Adding full bibliography for 7047755--7047762.cif.'
_cod_original_cell_volume        16401(5)
_cod_original_formula_sum        'C79.50 H110 Ce N19 Si2'
_cod_database_code               7047762
_shelx_estimated_absorpt_t_max   0.901
_shelx_estimated_absorpt_t_min   0.829
_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
 C37-C35 \\sim C37-C36 \\sim C35-C36
 with sigma of 0.04
 C7-C4 \\sim C7-C37 \\sim C7-C35 \\sim C7-C36
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C53) = Uanis(C47) = Uanis(C48) = Uanis(C49) = Uanis(C50) = Uanis(C51) =
Uanis(C52)
4. Others
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=
 Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=1-FVAR(1)
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(1)
 Sof(H12A)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C39)=Sof(H39A)=Sof(H39B)=
 Sof(H39C)=1-FVAR(2)
 Sof(H12)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=Sof(H14A)=Sof(H14B)=
 Sof(H14C)=FVAR(2)
 Sof(C61)=Sof(C62)=Sof(H62)=Sof(C63)=Sof(H63)=Sof(C64)=Sof(H64)=Sof(C65)=
 Sof(H65)=Sof(C66)=Sof(H66)=Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(H67C)=1-FVAR(3)
 Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(H60C)=Sof(C54)=Sof(C55)=Sof(H55)=Sof(C56)=
 Sof(H56)=Sof(C57)=Sof(H57)=Sof(C58)=Sof(H58)=Sof(C59)=Sof(H59)=FVAR(3)
 Fixed Sof: C53(0.5) H53A(0.5) H53B(0.5) H53C(0.5) C47(0.5) C48(0.5) H48(0.5)
 C49(0.5) H49(0.5) C50(0.5) H50(0.5) C51(0.5) H51(0.5) C52(0.5) H52(0.5)
5.a Free rotating group:
 C53(C47,C48,C49,C50,C51,C52), C60(C54,C55,C56,C57,C58,C59)
5.b Ternary CH refined with riding coordinates:
 C12(H12), C12(H12A), C26(H26), C12'(H12'), C26'(H26')
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C17(H17), C19(H19), C3'(H3'), C5'(H5'), C17'(H17'),
 C19'(H19'), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C55(H55),
 C56(H56), C57(H57), C58(H58), C59(H59), C40(H40), C41(H41), C42(H42), C44(H44),
  C45(H45), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66)
5.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C),
 C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,
 H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C8'(H8'A,H8'B,H8'C), C9'(H9'A,
 H9'B,H9'C), C10'(H10D,H10E,H10F), C13'(H13D,H13E,H13F), C14'(H14D,H14E,H14F),
 C22'(H22D,H22E,H22F), C23'(H23D,H23E,H23F), C24'(H24D,H24E,H24F), C27'(H27D,
 H27E,H27F), C28'(H28D,H28E,H28F), C53(H53A,H53B,H53C), C60(H60A,H60B,H60C),
 C46(H46A,H46B,H46C), C67(H67A,H67B,H67C)
;
_shelx_res_checksum              70814
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'