#------------------------------------------------------------------------------
#$Date: 2019-11-17 08:51:35 +0100 (dom 17 de nov de 2019) $
#$Revision: 229197 $
#$URL: svn://www.crystallography.net/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)
_iucr_refine_instructions_details
;
TITL
REM reset to Pnnm #58
REM pnnm in Pnnm #58
REM 42 parameters refined using 0 restraints
REM Highest difference peak 1.253, deepest hole -1.893, 1-sigma level 0.222
REM The information below was added by Olex2.
REM n/a parameters refined using n/a restraints
REM Highest difference peak 1.25, deepest hole -1.89
REM Mean Shift 0, Max Shift 0.000.
CELL 0.7109 7.687 18.84 4.189 90 90 90
ZERR 2 0.0015 0.0038 0.0008 0 0 0
LATT 1
SYMM -X,-Y,+Z
SYMM 0.5+X,0.5-Y,0.5-Z
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H Br O Yb
UNIT 16 32 4 4 2
 
L.S. 20
PLAN  20
SIZE 0.03 0.02 0.02
TEMP -173
GRID
BOND $H
fmap 2
acta
MERG 2
OMIT -2 54
REM <olex2.extras>
REM <HklSrc "%.\\pnnm.hkl">
REM </olex2.extras>
 
WGHT    0.000000    2.911200
EXTI    0.033108
FVAR       0.71680
YB1   5    0.500000    0.000000    0.000000    10.25000    0.02245    0.03004 =
         0.03683    0.00000    0.00000    0.00032
BR1   3    0.301113    0.067420   -0.500000    10.50000    0.02930    0.04297 =
         0.03986    0.00000    0.00000    0.00900
O1    4    0.693780    0.098446    0.000000    10.50000    0.02427    0.03528 =
         0.05663    0.00000    0.00000    0.00304
C1    1    0.883235    0.094231    0.000000    10.50000    0.02084    0.03997 =
         0.08087    0.00000    0.00000    0.00419
AFIX  23
H1A   2    0.924438    0.068550   -0.191824    10.50000   -1.20000
H1B   2    0.924438    0.068550    0.191824    10.50000   -1.20000
AFIX   0
C2    1    0.950419    0.167710    0.000000    10.50000    0.02952    0.03485 =
         0.08618    0.00000    0.00000    0.00060
AFIX  23
H2A   2    1.022820    0.176072   -0.191802    10.50000   -1.20000
H2B   2    1.022820    0.176072    0.191802    10.50000   -1.20000
AFIX   0
C3    1    0.798254    0.216102    0.000000    10.50000    0.03092    0.03739 =
         0.09975    0.00000    0.00000    0.00272
AFIX  23
H3A   2    0.800446    0.246790    0.191803    10.50000   -1.20000
H3B   2    0.800446    0.246790   -0.191803    10.50000   -1.20000
AFIX   0
C4    1    0.642942    0.172393    0.000000    10.50000    0.03245    0.02965 =
         0.12575    0.00000    0.00000    0.00612
AFIX  23
H4A   2    0.572011    0.182852    0.191570    10.50000   -1.20000
H4B   2    0.572011    0.182851   -0.191570    10.50000   -1.20000
HKLF 4
 
REM
REM R1 =  0.0388 for    673 Fo > 4sig(Fo)  and  0.0413 for all    732 data
REM     42 parameters refined using      0 restraints
 
END  
     
WGHT      0.0000      2.9134 
REM Highest difference peak  1.194,  deepest hole -1.650,  1-sigma level  0.197
Q1    1   0.5000  0.0000  0.1337  10.50000  0.05    1.19
Q2    1   0.5701  0.0461  0.0000  10.50000  0.05    1.19
Q3    1   0.2537  0.0175 -0.5000  10.50000  0.05    1.05
Q4    1   0.8020  0.2829  0.0000  10.50000  0.05    0.91
Q5    1   0.3697 -0.0481 -0.5000  10.50000  0.05    0.86
Q6    1   0.3872  0.1140 -0.5000  10.50000  0.05    0.62
Q7    1   0.3878  0.0263 -0.5000  10.50000  0.05    0.62
Q8    1   0.7799  0.0531 -0.5000  10.50000  0.05    0.61
Q9    1   0.9116  0.0667 -0.5000  10.50000  0.05    0.61
Q10   1   1.0726  0.1911  0.0000  10.50000  0.05    0.54
Q11   1   0.8964  0.0026  0.0000  10.50000  0.05    0.54
Q12   1   0.4470  0.0763 -0.5000  10.50000  0.05    0.51
Q13   1   0.5150  0.1734  0.0000  10.50000  0.05    0.49
Q14   1   0.3282  0.0441 -0.7100  11.00000  0.05    0.46
Q15   1   0.6126  0.1107  0.0000  10.50000  0.05    0.46
Q16   1   0.3431  0.0887 -0.7127  11.00000  0.05    0.43
Q17   1   0.8602  0.0981  0.2921  11.00000  0.05    0.42
Q18   1   0.4983  0.0794  0.2530  11.00000  0.05    0.42
Q19   1   0.4197  0.1125  0.0000  10.50000  0.05    0.41
Q20   1   0.1801  0.1231 -0.5000  10.50000  0.05    0.40

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0388 for 673 Fo > 4sig(Fo) and 0.0413 for all 5329 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 1.19, deepest hole -1.65
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0413
  REM R1_gt = 0.0388
  REM wR_ref = 0.0955
  REM GOOF = 1.068
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 5329
  REM Reflections_gt = 673
  REM Parameters = n/a
  REM Hole = -1.65
  REM Peak = 1.19
  REM Flack = n/a

  
;
_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_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Yb1 0.0224(4) 0.0300(4) 0.0368(4) 0.000 0.000 0.00032(18)
Br1 0.0293(5) 0.0430(6) 0.0399(5) 0.000 0.000 0.0090(4)
O1 0.024(3) 0.035(4) 0.057(4) 0.000 0.000 0.003(3)
C1 0.021(4) 0.040(5) 0.081(7) 0.000 0.000 0.004(4)
C2 0.030(4) 0.035(6) 0.086(8) 0.000 0.000 0.001(4)
C3 0.031(5) 0.037(6) 0.100(9) 0.000 0.000 0.003(4)
C4 0.032(5) 0.030(6) 0.126(11) 0.000 0.000 0.006(4)
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 .
