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_7116697
_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         'C76 H100 N4 Sm2, 4.5(C4 H8 O)'
_chemical_formula_sum            'C94 H136 N4 O4.5 Sm2'
_chemical_formula_weight         1694.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2014-12-11 deposited with the CCDC.
2015-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.3117(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.9726(2)
_cell_length_b                   18.7116(3)
_cell_length_c                   19.7467(3)
_cell_measurement_reflns_used    12143
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     4053.23(12)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997) & COLLECT'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        'DENZO & COLLECT'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    SHELXT(Sheldrick,2014)
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Kappa APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0678
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            56778
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         30.063
_diffrn_reflns_theta_min         2.152
_exptl_absorpt_coefficient_mu    1.490
_exptl_absorpt_correction_T_max  1.07681
_exptl_absorpt_correction_T_min  0.936131
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   DENZO/SCALEPACK
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_description       needle
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.912
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         11870
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0448P)^2^+8.1963P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1168
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9495
_reflns_number_total             11870
_reflns_threshold_expression     'I > 2\s(I)'
_cod_duplicate_entry             7116568
_cod_data_source_file            c5cc00289c2.cif
_cod_data_source_block           gnoc204_a_sq
_cod_original_formula_sum        'C94 H136 N4 O4.50 Sm2'
_cod_database_code               7116697
_shelx_estimated_absorpt_t_min   0.663
_shelx_estimated_absorpt_t_max   0.957
_shelxl_version_number           2014/6
_shelx_res_checksum              95303
_shelx_fab_checksum              17005