Unprecedented reaction of bridged bis(guanidinate) lanthanide complexes: sterically induced deprotonation.
Wang, Chuanyong; Zhang, Xingmin; Xue, Mingqiang; Zhang, Yong; Shen, Qi; Dalton transactions (Cambridge, England : 2003) 42 (2013) 7009–7018; doi:10.1039/c3dt32882a

data_7022712
_publ_section_title
;
 Unprecedented reaction of bridged bis(guanidinate) lanthanide complexes:
 sterically induced deprotonation.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7009
_journal_page_last               7018
_journal_paper_doi               10.1039/c3dt32882a
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C56 H86 N12 O2 Y2, 5(C4 H8 O)'
_chemical_formula_sum            'C76 H126 N12 O7 Y2'
_chemical_formula_weight         1497.71
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.244(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.2799(11)
_cell_length_b                   18.1316(7)
_cell_length_c                   16.7684(7)
_cell_measurement_reflns_used    6045
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      29.4252
_cell_measurement_theta_min      3.1647
_cell_volume                     8002.3(6)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      220(2)
_diffrn_detector_area_resol_mean 10.4692
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18163
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.17
_exptl_absorpt_coefficient_mu    1.500
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73019
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3200
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.659
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.076
_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     416
_refine_ls_number_reflns         7422
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0697P)^2^+14.2119P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1374
_reflns_number_gt                5618
_reflns_number_total             7422
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt32882a.txt
_cod_data_source_block           complex5
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7022712