#------------------------------------------------------------------------------
#$Date: 2016-03-21 06:11:35 +0100 (lun 21 de mar de 2016) $
#$Revision: 178552 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/59/4065924.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_4065924
loop_
_publ_author_name
'Rohr, Ahleah D.'
'Kampf, Jeff W.'
'Wolfe, John P.'
'Banaszak Holl, Mark M.'
_publ_section_title
;
 Parallelograms and Ladders: Polymorphic Solid-State Structures and
 Solution Equilibria of Cp*GeCl†
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5004
_journal_paper_doi               10.1021/om100198d
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C10 H15 Cl Ge'
_chemical_formula_sum            'C10 H15 Cl Ge'
_chemical_formula_weight         243.26
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00(3)
_cell_angle_beta                 102.54(3)
_cell_angle_gamma                90.00(3)
_cell_formula_units_Z            4
_cell_length_a                   9.0939(18)
_cell_length_b                   6.8790(14)
_cell_length_c                   17.395(4)
_cell_measurement_reflns_used    9994
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      29.76
_cell_measurement_theta_min      2.40
_cell_volume                     1062.2(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART-APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      85(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0134
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            50909
_diffrn_reflns_theta_full        29.65
_diffrn_reflns_theta_max         29.65
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    3.081
_exptl_absorpt_correction_T_max  0.4686
_exptl_absorpt_correction_T_min  0.3508
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;? 
  Blessing, R. Acta Cryst. (1995) A51 33-38.
  Sheldrick, G.  TWINABS  (Version 2008/1), Bruker AXS scaling and
  corrections for twinned crystals University of Gottingen, Germany 2008.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         2999
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0201
_refine_ls_R_factor_gt           0.0195
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0210P)²+0.7205P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0493
_refine_ls_wR_factor_ref         0.0495
_reflns_number_gt                2935
_reflns_number_total             2999
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100198d_si_001.cif
_cod_data_source_block           ar239
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4065924
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Cl1 Cl 0.76440(3) 0.78198(5) 0.080852(18) 0.01666(7) Uani 1 1 d .
Ge1 Ge 0.537246(14) 0.932767(19) 0.097957(7) 0.01247(5) Uani 1 1 d .
C1 C 0.43177(13) 0.66476(18) 0.13128(7) 0.0134(2) Uani 1 1 d .
C2 C 0.49864(14) 0.76908(18) 0.20207(7) 0.0140(2) Uani 1 1 d .
C3 C 0.29898(14) 0.76885(18) 0.09369(7) 0.0133(2) Uani 1 1 d .
C4 C 0.40216(14) 0.93181(18) 0.20800(7) 0.0146(2) Uani 1 1 d .
C5 C 0.28161(14) 0.93089(18) 0.14147(7) 0.0138(2) Uani 1 1 d .
C6 C 0.48055(15) 0.46796(19) 0.10942(8) 0.0183(2) Uani 1 1 d .
H6A H 0.4534 0.3699 0.1448 0.027 Uiso 1 1 calc R
H6B H 0.5899 0.4673 0.1142 0.027 Uiso 1 1 calc R
H6C H 0.4302 0.4380 0.0550 0.027 Uiso 1 1 calc R
C7 C 0.63161(15) 0.7006(2) 0.26323(8) 0.0199(3) Uani 1 1 d .
H7A H 0.6047 0.5815 0.2879 0.030 Uiso 1 1 calc R
H7B H 0.6605 0.8015 0.3034 0.030 Uiso 1 1 calc R
H7C H 0.7163 0.6741 0.2382 0.030 Uiso 1 1 calc R
C8 C 0.18982(15) 0.7126(2) 0.01911(8) 0.0193(2) Uani 1 1 d .
H8A H 0.0942 0.6725 0.0315 0.029 Uiso 1 1 calc R
H8B H 0.2316 0.6045 -0.0060 0.029 Uiso 1 1 calc R
H8D H 0.1725 0.8240 -0.0168 0.029 Uiso 1 1 calc R
C9 C 0.42549(17) 1.0748(2) 0.27463(8) 0.0209(3) Uani 1 1 d .
H9A H 0.3840 1.2013 0.2549 0.031 Uiso 1 1 calc R
H9D H 0.5335 1.0882 0.2973 0.031 Uiso 1 1 calc R
H9B H 0.3742 1.0285 0.3152 0.031 Uiso 1 1 calc R
C10 C 0.15658(15) 1.0763(2) 0.12126(9) 0.0197(3) Uani 1 1 d .
H10D H 0.1622 1.1669 0.1653 0.030 Uiso 1 1 calc R
H10A H 0.0595 1.0087 0.1112 0.030 Uiso 1 1 calc R
H10B H 0.1664 1.1486 0.0741 0.030 Uiso 1 1 calc 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
Cl1 0.01402(13) 0.01854(14) 0.01800(13) -0.00073(10) 0.00477(10) 0.00121(10)
Ge1 0.01413(7) 0.01123(7) 0.01240(7) 0.00090(4) 0.00365(5) -0.00008(4)
C1 0.0144(5) 0.0123(5) 0.0139(5) 0.0009(4) 0.0038(4) -0.0006(4)
C2 0.0147(5) 0.0151(5) 0.0124(5) 0.0020(4) 0.0035(4) -0.0008(4)
C3 0.0133(5) 0.0130(5) 0.0136(5) 0.0005(4) 0.0026(4) -0.0014(4)
C4 0.0154(5) 0.0156(6) 0.0139(5) -0.0008(4) 0.0059(4) -0.0022(4)
C5 0.0133(5) 0.0140(5) 0.0149(5) 0.0002(4) 0.0051(4) 0.0003(4)
C6 0.0210(6) 0.0116(5) 0.0224(6) 0.0004(5) 0.0049(5) 0.0012(5)
C7 0.0171(6) 0.0255(7) 0.0157(6) 0.0047(5) 0.0002(4) 0.0010(5)
C8 0.0182(6) 0.0207(6) 0.0169(6) -0.0022(5) -0.0007(4) -0.0015(5)
C9 0.0239(6) 0.0228(7) 0.0171(6) -0.0062(5) 0.0067(5) -0.0020(5)
C10 0.0167(6) 0.0195(6) 0.0243(6) 0.0004(5) 0.0071(5) 0.0042(5)
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 '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
C1 Ge1 C2 37.90(5)
C1 Ge1 Cl1 96.13(4)
C2 Ge1 Cl1 100.10(4)
C1 Ge1 C3 35.59(5)
C2 Ge1 C3 59.50(5)
Cl1 Ge1 C3 125.78(3)
C1 Ge1 C4 58.80(5)
C2 Ge1 C4 35.00(4)
Cl1 Ge1 C4 132.82(4)
C3 Ge1 C4 55.69(5)
C3 C1 C2 107.36(11)
C3 C1 C6 127.00(11)
C2 C1 C6 124.98(11)
C3 C1 Ge1 80.48(8)
C2 C1 Ge1 71.48(7)
C6 C1 Ge1 121.13(9)
C4 C2 C1 107.33(11)
C4 C2 C7 127.03(12)
C1 C2 C7 125.06(12)
C4 C2 Ge1 82.60(8)
C1 C2 Ge1 70.62(7)
C7 C2 Ge1 119.35(9)
C5 C3 C1 108.36(11)
C5 C3 C8 124.82(12)
C1 C3 C8 126.72(11)
C5 C3 Ge1 80.19(8)
C1 C3 Ge1 63.93(7)
C8 C3 Ge1 124.29(9)
C5 C4 C2 108.35(11)
C5 C4 C9 126.24(12)
C2 C4 C9 125.40(12)
C5 C4 Ge1 78.14(7)
C2 C4 Ge1 62.40(7)
C9 C4 Ge1 125.59(9)
C4 C5 C3 108.56(11)
C4 C5 C10 127.20(12)
C3 C5 C10 124.22(12)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Cl1 Ge1 2.3872(7)
Ge1 C1 2.2128(14)
Ge1 C2 2.2241(13)
Ge1 C3 2.4294(14)
Ge1 C4 2.4889(14)
C1 C3 1.4337(17)
C1 C2 1.4408(17)
C1 C6 1.4991(18)
C2 C4 1.4397(18)
C2 C7 1.5024(18)
C3 C5 1.4195(17)
C3 C8 1.5031(18)
C4 C5 1.4108(18)
C4 C9 1.4998(18)
C5 C10 1.4979(18)
