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_7047759
_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         'C112 H144 N36 O2 Sm2, 0.5(C7 H8)'
_chemical_formula_sum            'C115.5 H148 N36 O2 Sm2'
_chemical_formula_weight         2373.39
_chemical_melting_point          ?
_chemical_name_common            '[Sm(CzTiPr)2]2(mu-OH)2'
_chemical_name_systematic
Sm(\k3-CzTiPr)(\k3-\m-CzTiPr)(\m-OH)2Sm(\k3-CzTiPr)(\k2-CzTiPr)
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2018-07-04 deposited with the CCDC.
2018-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                73.382(3)
_cell_angle_beta                 72.642(3)
_cell_angle_gamma                89.771(3)
_cell_formula_units_Z            2
_cell_length_a                   16.4900(19)
_cell_length_b                   19.382(2)
_cell_length_c                   21.328(2)
_cell_measurement_reflns_used    9874
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      35.14
_cell_measurement_theta_min      2.38
_cell_volume                     6209.7(11)
_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    'Bruker XP (Bruker, 2015)'
_computing_publication_material  'CIFTAB (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2014/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker PHOTON-100 CMOS'
_diffrn_measurement_method       'combination of \w and \f-scans '
_diffrn_radiation_monochromator  'multi-layer toroidal'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.0332
_diffrn_reflns_av_R_equivalents  0.1086
_diffrn_reflns_av_unetI/netI     0.1255
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            50956
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        35.632
_diffrn_reflns_theta_max         35.632
_diffrn_reflns_theta_min         2.365
_exptl_absorpt_coefficient_mu    2.746
_exptl_absorpt_correction_T_max  0.4370
_exptl_absorpt_correction_T_min  0.2586
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_description       tablet
_exptl_crystal_F_000             2466
_exptl_crystal_recrystallization_method
'Hydrolysis byproduct of Sm(CzTiPr)2[N(SiMe3)2]'
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_refine_diff_density_max         2.607
_refine_diff_density_min         -1.373
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1371
_refine_ls_number_reflns         18131
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1436
_refine_ls_R_factor_gt           0.0932
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1706P)^2^+3.0948P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2425
_refine_ls_wR_factor_ref         0.2805
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11342
_reflns_number_total             18131
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02757a2.cif
_cod_data_source_block           uvic005
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'unknown' was changed to '?' - the
value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7047755--7047762.cif.
;
_cod_original_cell_volume        6209.8(12)
_cod_original_formula_sum        'C115.50 H148 N36 O2 Sm2'
_cod_database_code               7047759
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.875
_shelx_estimated_absorpt_t_max   0.973
_shelx_res_checksum              77969