Synthesis of Unsupported Ln‒Ga Bonds by Salt Metathesis and Ga‒Ga Bond Reduction
Sanden, Tanja; Gamer, Michael T.; Fagin, Anatoly A.; Chudakova, Valentina A.; Konchenko, Sergey N.; Fedushkin, Igor L.; Roesky, Peter W.; Organometallics 31 (2012) 4331–; doi:10.1021/om300309b

data_4078541
_publ_section_title
;
 Synthesis of Unsupported Ln--Ga Bonds by Salt Metathesis and Ga--Ga Bond
 Reduction
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              4331
_journal_paper_doi               10.1021/om300309b
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C88 H112 Ga2 N4 O4 Sm, 2(C4 H8 O), C7 H8'
_chemical_formula_sum            'C103 H136 Ga2 N4 O6 Sm'
_chemical_formula_weight         1815.95
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 99.393(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.7406(7)
_cell_length_b                   15.4964(5)
_cell_length_c                   24.3631(11)
_cell_measurement_reflns_used    14943
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.51
_cell_measurement_theta_min      1.56
_cell_volume                     4745.6(4)
_computing_cell_refinement       'STOE X-AREA, PLATON (A.L.Spek, 2005)'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED, PLATON (A.L.Spek, 2005)'
_computing_molecular_graphics
;
Diamond 2.1e/3

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.

Microsoft Word
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0483
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18069
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    1.228
_exptl_absorpt_correction_T_max  0.8714
_exptl_absorpt_correction_T_min  0.7332
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1908
_exptl_crystal_size_max          0.302
_exptl_crystal_size_mid          0.247
_exptl_crystal_size_min          0.202
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.910
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         8536
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.911
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0749
_reflns_number_gt                6215
_reflns_number_total             8536
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300309b_si_002.cif
_cod_data_source_block           1'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4078541