Reversible C‒C coupling in phenanthroline complexes of divalent samarium and thulium
Nocton, Grégory; Ricard, Louis; Chemical Communications (Cambridge, United Kingdom) 51 (2015) 3578–3581; doi:10.1039/c5cc00289c

data_7116696
_publ_section_title
;
 Reversible C--C coupling in phenanthroline complexes of divalent
 samarium and thulium
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   17
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              3578
_journal_page_last               3581
_journal_paper_doi               10.1039/c5cc00289c
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C92 H132 N4 Sm2, 2(C7H8)'
_chemical_formula_sum            'C120 H164 N4 Sm2'
_chemical_formula_weight         1963.24
_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
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-12-11 deposited with the CCDC.
2015-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                87.677(1)
_cell_angle_beta                 87.886(1)
_cell_angle_gamma                83.688(1)
_cell_formula_units_Z            1
_cell_length_a                   10.225(1)
_cell_length_b                   12.304(1)
_cell_length_c                   20.627(1)
_cell_measurement_reflns_used    4590
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     2575.8(4)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_Laue_measured_fraction_full 0.957
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18460
_diffrn_reflns_point_group_measured_fraction_full 0.957
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         27.456
_diffrn_reflns_theta_min         1.968
_exptl_absorpt_coefficient_mu    1.179
_exptl_absorpt_correction_T_max  1.36889
_exptl_absorpt_correction_T_min  0.758813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   DENZO/SCALEPACK
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_description       plate
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_platon_squeeze_details
;
Two toluene molecules were located in the unit cell but could not be modelled
adequately. SQUEEZE was used to remove these contributions from the structure
factors.
;
_refine_diff_density_max         1.163
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         11083
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0534P)^2^+9.3526P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1387
_refine_ls_wR_factor_ref         0.1456
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9882
_reflns_number_total             11083
_reflns_threshold_expression     'I > 2\s(I)'
_cod_duplicate_entry             7116567
_cod_data_source_file            c5cc00289c2.cif
_cod_data_source_block           gno95_sq_s
_cod_database_code               7116696
_shelx_estimated_absorpt_t_min   0.933
_shelx_estimated_absorpt_t_max   0.977
_shelxl_version_number           2013-4
_shelx_res_checksum              28096
_shelx_fab_checksum              19706