Exploring secondary bonding in p-block chemistry – an experimental study of [GeX2{o-C6H4(PMe2)2}] using variable pressure single crystal X-ray diffraction
Allan, David R.; Coles, Simon J.; George, Kathryn; Jura, Marek; Levason, William; Reid, Gillian; Wilson, Claire; Zhang, Wenjian; CrystEngComm 16 (2014) 8169–; doi:10.1039/C4CE00329B

data_7217978
_publ_section_title
;
 Exploring secondary bonding in p-block chemistry -- an experimental study
 of [GeX2{o-C6H4(PMe2)2}] using variable pressure single crystal X-ray
 diffraction
;
_journal_issue                   35
_journal_name_full               CrystEngComm
_journal_page_first              8169
_journal_paper_doi               10.1039/C4CE00329B
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C10 H16 Cl2 Ge P2'
_chemical_formula_sum            'C10 H16 Cl2 Ge P2'
_chemical_formula_weight         341.66
_chemical_name_systematic
;
Dichlorido(1,2-bis(dimethylphosphino)benzene)germanium(II)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-11-23
_audit_creation_method
;
  Olex2 1.2
  (compiled Nov  5 2012 18:25:38, GUI svn.r4372)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 110.00(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.691(16)
_cell_length_b                   7.225(3)
_cell_length_c                   13.704(4)
_cell_measurement_pressure       1400000
_cell_measurement_reflns_used    812
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.4
_cell_measurement_theta_min      2.0
_cell_volume                     2576(2)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2011)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_pressure         1400000
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.434
_diffrn_measured_fraction_theta_max 0.434
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_type  CrystalLogic
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Diamond Anvil Cell'
_diffrn_radiation_collimation    'Confocal mirrors'
_diffrn_radiation_monochromator  'double crystal silicon'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.48590
_diffrn_reflns_av_R_equivalents  0.2256
_diffrn_reflns_av_unetI/netI     0.1529
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8513
_diffrn_reflns_theta_full        18.56
_diffrn_reflns_theta_max         18.56
_diffrn_reflns_theta_min         2.00
_diffrn_source                   synchrotron
_diffrn_source_type              'DLS beamline I19'
_exptl_absorpt_coefficient_mu    1.054
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.863
_refine_diff_density_min         -1.055
_refine_diff_density_rms         0.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         1319
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.1954
_refine_ls_R_factor_gt           0.1138
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0721P)^2^+171.5618P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2252
_refine_ls_wR_factor_ref         0.2981
_reflns_number_gt                838
_reflns_number_total             1319
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c4ce00329b2.cif
_cod_data_source_block           gecl2diphos2
_cod_database_code               7217978
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H5 of C5, H4 of C4, H6 of C6, H7 of C7
 At 1.5 times of:
  {H9A,H9B,H9C} of C9, {H2A,H2B,H2C} of C2, {H1A,H1B,H1C} of C1, {H10A,H10B,
  H10C} of C10
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7)
2.b Fitted hexagon refined as free rotating group:
 C3(C4,C5,C6,C7,C8)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;