A base-free synthetic route to anti-bimetallic lanthanide pentalene complexes.
Kilpatrick, Alexander F. R.; Cloke, F Geoffrey N; Dalton transactions (Cambridge, England : 2003) 46 (2017) 5587–5597; doi:10.1039/c6dt04475a

data_7041560
_publ_section_title
;
 A base-free synthetic route to anti-bimetallic lanthanide pentalene
 complexes.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5587
_journal_page_last               5597
_journal_paper_doi               10.1039/c6dt04475a
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C46 H76 Eu2 Si2, C7 H8'
_chemical_formula_sum            'C53 H84 Eu2 Si2'
_chemical_formula_weight         1081.30
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-12-19
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2016-12-19 deposited with the CCDC.
2016-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.8178(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8290(3)
_cell_length_b                   15.4443(2)
_cell_length_c                   20.1752(3)
_cell_measurement_reflns_used    17912
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.3570
_cell_measurement_theta_min      3.1960
_cell_volume                     5166.98(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material
;
OLEX2 (Dolomanov et al, 2009), SHELXL-2013 (Sheldrick, 2013), 
PLATON (Spek, 2003), WinGX (Farrugia, 2013)
;
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0804
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31348
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.404
_diffrn_reflns_theta_min         3.751
_exptl_absorpt_coefficient_mu    17.864
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36396
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.778
_refine_diff_density_min         -1.751
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         9914
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0532
_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^)+(0.0845P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1262
_refine_ls_wR_factor_ref         0.1308
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8937
_reflns_number_total             9914
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04475a2.cif
_cod_data_source_block           Compound2
_cod_depositor_comments
'Adding full bibliography for 7041560--7041563.cif.'
_cod_original_cell_volume        5166.99(15)
_cod_database_code               7041560
_shelx_estimated_absorpt_t_max   0.075
_shelx_estimated_absorpt_t_min   0.041
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C18(H18), C21(H21), C24(H24), C9(H9), C15(H15), C12(H12)
2.b Me refined with riding coordinates:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C23(H23A,H23B,H23C), C22(H22A,H22B,
 H22C), C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C11(H11A,H11B,H11C), C10(H10A,
 H10B,H10C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C14(H14A,H14B,H14C),
 C13(H13A,H13B,H13C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,
 H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C), C36(H36A,H36B,H36C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C),
 C53(H53A,H53B,H53C)
2.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C3(H3), C2(H2), C51(H51), C52(H52), C47(H47), C48(H48),
 C49(H49)
;
_shelx_shelxl_version_number     2016/4
_olex2_submission_special_instructions 'No special instructions were received'