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_7047755
_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         'C28 H37 N9, 0.5(C3 H8 O)'
_chemical_formula_sum            'C29.5 H41 N9 O0.5'
_chemical_formula_weight         529.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-09-18
_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                90
_cell_angle_beta                 104.335(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5895(14)
_cell_length_b                   18.322(2)
_cell_length_c                   14.4238(18)
_cell_measurement_reflns_used    7634
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.64
_cell_measurement_theta_min      2.31
_cell_volume                     2967.4(6)
_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  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      90.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0468
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29581
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.806
_diffrn_reflns_theta_min         1.833
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0786 before and 0.0507 after correction.
The Ratio of minimum to maximum transmission is 0.9265.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_description       prism
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         7007
_refine_ls_number_restraints     77
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0903
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0715P)^2^+0.7222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1350
_refine_ls_wR_factor_ref         0.1550
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4652
_reflns_number_total             7007
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02757a2.cif
_cod_data_source_block           Compound_2
_cod_depositor_comments
'Adding full bibliography for 7047755--7047762.cif.'
_cod_original_cell_volume        2967.5(6)
_cod_original_formula_sum        'C29.50 H41 N9 O0.50'
_cod_database_code               7047755
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.987
_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, All O(H) groups
2. Restrained distances
 C24-C25 = C26-C25
 1.5 with sigma of 0.01
 C8'-C10' \\sim C8'-C9' \\sim C10'-C9' \\sim C19-C20 \\sim C19-C21 \\sim C20-C21
 with sigma of 0.04
 C18-C4' \\sim C18-C8' \\sim C18-C10' \\sim C18-C9' \\sim C18-C19 \\sim C18-C20
\\sim C18-C21
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C18, C19, C20, C21, C4'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, C25, C24
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=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(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=
 Sof(H12A)=1-FVAR(2)
 Sof(H12')=Sof(C13')=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C14')=Sof(H14D)=
 Sof(H14E)=Sof(H14F)=FVAR(2)
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=1-FVAR(3)
 Sof(C8')=Sof(H8'A)=Sof(H8'B)=Sof(H8'C)=Sof(C9')=Sof(H9'A)=Sof(H9'B)=Sof(H9'C)=
 Sof(C10')=Sof(H10D)=Sof(H10E)=Sof(H10F)=FVAR(3)
 Fixed Sof: O1(0.5) H1A(0.5) C25(0.5) H25(0.5) C24(0.5) H24A(0.5) H24B(0.5)
 H24C(0.5) C26(0.5) H26A(0.5) H26B(0.5) H26C(0.5)
5.a Ternary CH refined with riding coordinates:
 C12(H12), C12'(H12'), C12'(H12A), C25(H25)
5.b Me refined with riding coordinates:
 C24(H24A,H24B,H24C), C26(H26A,H26B,H26C)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C3'(H3'), C5'(H5')
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), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,
 H22B,H22C), C23(H23A,H23B,H23C), 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)
5.e Idealised tetrahedral OH refined as rotating group:
 O1(H1A)
;
_shelx_res_checksum              39550
_olex2_submission_special_instructions 'No special instructions were received'