Half-sandwich bis(propiolamidinate) rare-earth metal complexes: synthesis, structure and dissociation of the cyclopentadienyl ligand via competition with an amidinate.
Xu, Ling; Wang, Yu-Chen; Zhang, Wen-Xiong; Xi, Zhenfeng; Dalton transactions (Cambridge, England : 2003) 42 (2013) 16466–16469; doi:10.1039/c3dt52179f

data_7023972
_publ_section_title
;
 Half-sandwich bis(propiolamidinate) rare-earth metal complexes:
 synthesis, structure and dissociation of the cyclopentadienyl ligand via
 competition with an amidinate.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16466
_journal_page_last               16469
_journal_paper_doi               10.1039/c3dt52179f
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C45 H57 N6 Y1'
_chemical_formula_sum            'C45 H57 N6 Y'
_chemical_formula_weight         770.87
_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_Hall           'P 6c'
_space_group_name_H-M_alt        'P 63'
_symmetry_space_group_name_Hall  'P 6c'
_symmetry_space_group_name_H-M   'P 63'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2013-09-14
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   16.124(2)
_cell_length_b                   16.124(2)
_cell_length_c                   9.945(2)
_cell_measurement_temperature    173(2)
_cell_volume                     2239.1(6)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0760
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            14012
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         2.526
_exptl_absorpt_coefficient_mu    1.337
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.113(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         2910
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0536
_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^)+(0.0387P)^2^+1.5495P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1142
_reflns_Friedel_coverage         0.887
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                2764
_reflns_number_total             2910
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt52179f.txt
_cod_data_source_block           a
_cod_original_cell_volume        2239.1(8)
_cod_database_code               7023972
_olex2_refinement_description
;
1. Others
 Fixed U13: Y1(0)
 Fixed U23: Y1(0)
 Fixed Uiso: H1(0.056) H2A(0.139) H2B(0.139) H2C(0.139) H3A(0.1) H3B(0.1)
 H3C(0.1) H4(0.059) H5A(0.154) H5B(0.154) H5C(0.154) H6A(0.143) H6B(0.143)
 H6C(0.143) H11(0.097) H12(0.127) H13(0.124) H14(0.104) H15(0.077)
 Fixed X: Y1(0.3333) H1(0.2129) H2A(0.3306) H2B(0.228) H2C(0.2801) H3A(0.1337)
 H3B(0.0862) H3C(0.0948) H4(0.3836) H5A(0.3284) H5B(0.4312) H5C(0.4218)
 H6A(0.5482) H6B(0.5219) H6C(0.5408) H11(0.1802) H12(0.1489) H13(0.2093)
 H14(0.3051) H15(0.3348)
 Fixed Y: Y1(0.6667) H1(0.3879) H2A(0.4921) H2B(0.449) H2C(0.5557) H3A(0.5099)
 H3B(0.4045) H3C(0.4187) H4(0.4567) H5A(0.5304) H5B(0.5493) H5C(0.6321)
 H6A(0.5605) H6B(0.5499) H6C(0.6439) H11(0.1682) H12(0.0093) H13(-0.043)
 H14(0.0628) H15(0.2198)
 Fixed Z: H1(0.8353) H2A(0.9846) H2B(1.0551) H2C(0.9964) H3A(0.8569)
 H3B(0.9196) H3C(0.76) H4(0.4322) H5A(0.2832) H5B(0.2353) H5C(0.3103)
 H6A(0.4022) H6B(0.5588) H6C(0.4787) H11(0.4695) H12(0.4732) H13(0.6419)
 H14(0.8073) H15(0.8112)
;
_shelx_estimated_absorpt_t_max   0.805
_shelx_estimated_absorpt_t_min   0.767
_shelx_hkl_checksum              94090
_shelx_res_checksum              54061
_shelxl_version_number           2013-3