#------------------------------------------------------------------------------
#$Date: 2019-11-17 09:51:35 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229197 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/68/7046814.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7046814
loop_
_publ_author_name
'de Bruin-Dickason, Caspar N'
'Boutland, Aaron J.'
'Dange, Deepak'
'Deacon, Glen B.'
'Jones, Cameron'
_publ_section_title
;
 Redox transmetallation approaches to the synthesis of extremely bulky
 amido-lanthanoid(ii) and -calcium(ii) complexes.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9512
_journal_page_last               9520
_journal_paper_doi               10.1039/c8dt02138d
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C8 H16 Br2 O2 Yb'
_chemical_formula_sum            'C8 H16 Br2 O2 Yb'
_chemical_formula_weight         477.07
_space_group_crystal_system      orthorhombic
_space_group_IT_number           58
_space_group_name_Hall           '-P 2 2n'
_space_group_name_H-M_alt        'P n n m'
_symmetry_space_group_name_Hall  '-P 2 2n'
_symmetry_space_group_name_H-M   'P n n m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-03-02
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-05-25 deposited with the CCDC.
2018-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.6870(15)
_cell_length_b                   18.840(4)
_cell_length_c                   4.1890(8)
_cell_measurement_reflns_used    4674
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.99
_cell_measurement_theta_min      3.42
_cell_volume                     606.7(2)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Australian Synchrotron'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.71090
_diffrn_reflns_av_R_equivalents  0.1546
_diffrn_reflns_av_unetI/netI     0.0789
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            4674
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         3.42
_diffrn_source                   'Australian Synchrotron'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.264
_exptl_absorpt_correction_T_max  0.7635
_exptl_absorpt_correction_T_min  0.6742
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XScale within XDS'
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.612
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.194
_refine_diff_density_min         -1.650
_refine_diff_density_rms         0.197
_refine_ls_extinction_coef       0.033(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         732
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+2.9112P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.0955
_reflns_number_gt                673
_reflns_number_total             732
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8dt02138d2.cif
_cod_data_source_block           compound2S
_cod_depositor_comments
'Adding full bibliography for 7046810--7046818.cif.'
_cod_database_code               7046814
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Others
 Fixed Sof: H1A(0.5) H1B(0.5) H2A(0.5) H2B(0.5) H3A(0.5) H3B(0.5) H4A(0.5)
 H4B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, z'
3 'x+1/2, -y+1/2, -z+1/2'
4 '-x+1/2, y+1/2, -z+1/2'
5 '-x, -y, -z'
6 'x, y, -z'
7 '-x-1/2, y-1/2, z-1/2'
8 'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Yb1 Yb 0.5000 0.0000 0.0000 0.0298(3) Uani 1 d 4 S T P
Br1 Br 0.30111(12) 0.06742(5) -0.5000 0.0374(3) Uani 1 d 2 S T P
O1 O 0.6938(8) 0.0984(4) 0.0000 0.0387(15) Uani 1 d 2 S T P
C1 C 0.8832(12) 0.0942(6) 0.0000 0.047(3) Uani 1 d 2 S T P
H1A H 0.9244 0.0686 -0.1918 0.057 Uiso 0.50 calc 1 R . .
H1B H 0.9244 0.0686 0.1918 0.057 Uiso 0.50 calc 1 R . .
C2 C 0.9504(13) 0.1677(6) 0.0000 0.050(3) Uani 1 d 2 S T P
H2A H 1.0228 0.1761 -0.1918 0.060 Uiso 0.50 calc 1 R . .
H2B H 1.0228 0.1761 0.1918 0.060 Uiso 0.50 calc 1 R . .
C3 C 0.7983(13) 0.2161(6) 0.0000 0.056(3) Uani 1 d 2 S T P
H3A H 0.8004 0.2468 0.1918 0.067 Uiso 0.50 calc 1 R . .
H3B H 0.8004 0.2468 -0.1918 0.067 Uiso 0.50 calc 1 R . .
C4 C 0.6429(13) 0.1724(6) 0.0000 0.063(4) Uani 1 d 2 S T P
H4A H 0.5720 0.1829 0.1916 0.075 Uiso 0.50 calc 1 R . .
H4B H 0.5720 0.1829 -0.1916 0.075 Uiso 0.50 calc 1 R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
Yb1 Yb1 Yb1 180.0 1_554 1_556
Br1 Yb1 Yb1 136.499(15) 1_556 1_554
Br1 Yb1 Yb1 43.501(15) 5_655 1_556
Br1 Yb1 Yb1 43.501(15) . 1_554
Br1 Yb1 Yb1 136.499(15) . 1_556
Br1 Yb1 Yb1 136.499(15) 5_654 1_556
Br1 Yb1 Yb1 43.501(15) 1_556 1_556
Br1 Yb1 Yb1 43.501(15) 5_654 1_554
Br1 Yb1 Yb1 136.499(15) 5_655 1_554
Br1 Yb1 Br1 87.00(3) 5_655 1_556
Br1 Yb1 Br1 93.00(3) . 1_556
Br1 Yb1 Br1 93.00(3) 5_655 5_654
Br1 Yb1 Br1 180.0 . 5_655
Br1 Yb1 Br1 87.00(3) . 5_654
Br1 Yb1 Br1 180.00(5) 5_654 1_556
O1 Yb1 Yb1 90.0 . 1_554
O1 Yb1 Yb1 90.0 . 1_556
O1 Yb1 Yb1 90.0 5_655 1_554
O1 Yb1 Yb1 90.0 5_655 1_556
O1 Yb1 Br1 90.66(11) . 5_655
O1 Yb1 Br1 90.66(11) 5_655 1_556
O1 Yb1 Br1 89.34(11) 5_655 5_655
O1 Yb1 Br1 89.34(11) . .
O1 Yb1 Br1 90.66(11) 5_655 .
O1 Yb1 Br1 89.34(11) 5_655 5_654
O1 Yb1 Br1 90.66(11) . 5_654
O1 Yb1 Br1 89.34(11) . 1_556
O1 Yb1 O1 180.0 . 5_655
Yb1 Br1 Yb1 93.00(3) . 1_554
C1 O1 Yb1 125.6(6) . .
C4 O1 Yb1 125.6(6) . .
C4 O1 C1 108.8(7) . .
O1 C1 H1A 110.2 . .
O1 C1 H1B 110.2 . .
O1 C1 C2 107.3(8) . .
H1A C1 H1B 108.5 . .
C2 C1 H1A 110.2 . .
C2 C1 H1B 110.2 . .
C1 C2 H2A 110.2 . .
C1 C2 H2B 110.2 . .
C1 C2 C3 107.5(8) . .
H2A C2 H2B 108.5 . .
C3 C2 H2A 110.2 . .
C3 C2 H2B 110.2 . .
C2 C3 H3A 110.2 . .
C2 C3 H3B 110.2 . .
H3A C3 H3B 108.5 . .
C4 C3 C2 107.5(9) . .
C4 C3 H3A 110.2 . .
C4 C3 H3B 110.2 . .
O1 C4 C3 108.9(8) . .
O1 C4 H4A 109.9 . .
O1 C4 H4B 109.9 . .
C3 C4 H4A 109.9 . .
C3 C4 H4B 109.9 . .
H4A C4 H4B 108.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Yb1 Yb1 4.1890(8) 1_556
Yb1 Yb1 4.1890(8) 1_554
Yb1 Br1 2.8875(7) 5_654
Yb1 Br1 2.8875(7) 5_655
Yb1 Br1 2.8875(7) .
Yb1 Br1 2.8875(7) 1_556
Yb1 O1 2.379(7) 5_655
Yb1 O1 2.379(7) .
Br1 Yb1 2.8875(7) 1_554
O1 C1 1.459(10) .
O1 C4 1.447(12) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C1 C2 1.478(15) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C2 C3 1.483(14) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C3 C4 1.450(14) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
