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_7217987
_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 Br2 Ge P2'
_chemical_formula_sum            'C10 H16 Br2 Ge P2'
_chemical_formula_weight         430.58
_chemical_name_systematic
;
 Dibromo(1,2-bis(dimethylphosphino)benzene-P,P')germanium(II)
;
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_symmetry_cell_setting           monoclinic
_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             2013-01-24
_audit_creation_method           'SHELXL-97 + hand edit'
_cell_angle_alpha                90.00
_cell_angle_beta                 92.25(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.773(10)
_cell_length_b                   6.98(3)
_cell_length_c                   13.67(5)
_cell_measurement_pressure       5400000
_cell_measurement_reflns_used    410
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.4
_cell_measurement_theta_min      2.9
_cell_volume                     2362(13)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_pressure         5400000
_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 0.291
_diffrn_measured_fraction_theta_max 0.291
_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     0.68890
_diffrn_reflns_av_R_equivalents  0.0979
_diffrn_reflns_av_sigmaI/netI    0.0916
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4347
_diffrn_reflns_theta_full        28.65
_diffrn_reflns_theta_max         28.65
_diffrn_reflns_theta_min         2.89
_diffrn_source                   synchrotron
_diffrn_source_type              'DLS beamline I19'
_exptl_absorpt_coefficient_mu    8.845
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.582
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.929
_refine_diff_density_min         -0.929
_refine_diff_density_rms         0.228
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     64
_refine_ls_number_reflns         970
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1576
_refine_ls_R_factor_gt           0.1077
_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/[\s^2^(Fo^2^)+(0.0449P)^2^+432.9641P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2252
_refine_ls_wR_factor_ref         0.2628
_reflns_number_gt                649
_reflns_number_total             970
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            c4ce00329b2.cif
_cod_data_source_block           gebr2diphos6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7217987