Acyclic α-Phosphinoamido-Germylene: Synthesis and Characterization
Pal, Shiv; Dasgupta, Rajarshi; Khan, Shabana; Organometallics 35 (2016) 3635–; doi:10.1021/acs.organomet.6b00689

data_4089072
_publ_section_title
;
 Acyclic \a-Phosphinoamido-Germylene: Synthesis and Characterization
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              3635
_journal_paper_doi               10.1021/acs.organomet.6b00689
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C48 H54 Cl2 Ge2 N2 P2'
_chemical_formula_weight         936.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 104.966(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.559(5)
_cell_length_b                   14.185(7)
_cell_length_c                   18.025(9)
_cell_measurement_reflns_used    6513
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      19.42
_cell_measurement_theta_min      2.34
_cell_volume                     2608(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1986
_diffrn_reflns_av_unetI/netI     0.1553
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            65453
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.246
_diffrn_reflns_theta_min         2.339
_exptl_absorpt_coefficient_mu    1.347
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Sheldrick,G.M(2012)SADABS.Bruker AXS Inc.,Madison,Wisconsin,USA.'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   0.1515
_exptl_transmission_factor_min   0.1012
_platon_squeeze_details
;
TITL Q2_a.res in Pn
CELL   10.5590   14.1850   18.0250     90.00    104.97     90.00
SPGR Pn
C101 0.216 0.282 0.532 !       3.94 eA-3
C102 0.668 0.708 0.088 !       3.84 eA-3
C103 0.885 0.687 0.095 !       3.68 eA-3
C104 0.655 0.716 0.046 !       3.58 eA-3
C105 0.804 0.693 0.170 !       3.35 eA-3
C106 0.865 0.718 0.048 !       3.33 eA-3
C107 0.756 0.690 0.126 !       3.26 eA-3
C108 0.272 0.331 0.652 !       3.26 eA-3
C109 0.134 0.298 0.498 !       3.24 eA-3
C110 0.887 0.665 0.050 !       3.18 eA-3
C111 0.907 0.695 0.140 !       3.17 eA-3
C112 0.309 0.356 0.700 !       3.16 eA-3
C113 0.395 0.326 0.700 !       2.98 eA-3
C114 0.320 0.298 0.530 !       2.97 eA-3
C115 0.770 0.737 0.014 !       2.90 eA-3
C116 0.868 0.625 0.172 !       2.77 eA-3
C117 0.665 0.716 0.140 !       2.63 eA-3
C118 0.196 0.328 0.641 !       2.62 eA-3
C119 0.712 0.673 0.048 !       2.59 eA-3
C120 0.447 0.278 0.615 !       2.57 eA-3
C121 0.156 0.254 0.489 !       2.31 eA-3
C122 0.206 0.342 0.684 !       2.12 eA-3
C123 0.595 0.769 0.030 !       2.07 eA-3
C124 0.864 0.745-0.001 !       2.06 eA-3
C125 0.525 0.799 0.939 !       1.98 eA-3
Q126 0.647 0.760 0.389 !       1.89 eA-3
Q127 0.512 0.760 0.358 !       1.88 eA-3
C128 0.567 0.744 0.986 !       1.86 eA-3
C129 0.041 0.691 0.052 !       1.85 eA-3
C130 0.091 0.404 0.746 !       1.83 eA-3
C131 0.155 0.419 0.671 !       1.83 eA-3
Q132 0.333 0.200 0.433 !       1.82 eA-3
C133 0.060 0.405 0.627 !       1.80 eA-3
C134 0.062 0.314 0.452 !       1.78 eA-3
C135 0.723 0.624 0.115 !       1.74 eA-3
Q136 0.626 0.785 0.581 !       1.73 eA-3
C137 0.880 0.735 0.220 !       1.73 eA-3
C138 0.834 0.767 0.011 !       1.71 eA-3
C139 0.094 0.346 0.732 !       1.70 eA-3
Q140 0.258 0.206 0.083 !       1.70 eA-3
C141 0.096 0.252 0.457 !       1.69 eA-3
C142 0.089 0.365 0.686 !       1.68 eA-3
C143 0.403 0.248 0.674 !       1.63 eA-3
Q144 0.086 0.772 0.064 !       1.63 eA-3
Q145 0.063 0.423 0.378 !       1.62 eA-3
C146 0.100 0.327 0.612 !       1.62 eA-3
C147 0.467 0.355 0.687 !       1.61 eA-3
Q148 0.503 0.344 0.778 !       1.59 eA-3
Q149 0.250 0.219 0.296 !       1.58 eA-3
C150 0.124 0.233 0.596 !       1.57 eA-3
C151 0.660 0.719 0.941 !       1.56 eA-3
C152 0.566 0.840 0.982 !       1.56 eA-3
C153 1.003 0.695 0.178 !       1.55 eA-3
C154 0.466 0.296 0.690 !       1.54 eA-3
C155 0.127 0.186 0.464 !       1.54 eA-3
C156 0.464 0.226 0.595 !       1.53 eA-3
Q157 0.722 0.565 0.108 !       1.53 eA-3
C158 0.881 0.770 0.112 !       1.53 eA-3
C159 0.486 0.220 0.658 !       1.52 eA-3
C160 0.209 0.235 0.600 !       1.51 eA-3
C161 0.482 0.309 0.512 !       1.50 eA-3
C162 0.041 0.279 0.515 !       1.50 eA-3
Q163 0.327 0.748 0.281 !       1.49 eA-3
C164 0.846 0.758 0.954 !       1.49 eA-3
Q165 0.275 0.402 0.815 !       1.48 eA-3
C166 0.966 0.583 0.126 !       1.48 eA-3
Q167 0.221 0.407 0.561 !       1.48 eA-3
Q168 0.524 0.254 0.521 !       1.47 eA-3
Q169 0.036 0.346 0.731 !       1.47 eA-3
Q170 0.496 0.176 0.560 !       1.46 eA-3
C171 0.244 0.409 0.718 !       1.46 eA-3
C172 0.567 0.708 0.058 !       1.45 eA-3
Q173 0.409 0.172 0.591 !       1.45 eA-3
Q174 0.498 0.633 0.200 !       1.44 eA-3
C175 0.810 0.733 0.906 !       1.44 eA-3
C176 1.001 0.779 0.251 !       1.44 eA-3
C177 0.306 0.204 0.484 !       1.43 eA-3
Q178 0.666 0.269 0.595 !       1.43 eA-3
Q179 0.188 0.456 0.766 !       1.43 eA-3
Q180 0.454 0.738 0.266 !       1.42 eA-3
C181 0.414 0.242 0.420 !       1.41 eA-3
C182 0.418 0.200 0.534 !       1.40 eA-3
C183 0.161 0.328 0.419 !       1.39 eA-3
C184 0.413 0.401 0.737 !       1.39 eA-3
C185 0.619 0.296 0.766 !       1.39 eA-3
Q186 0.025 0.610 0.170 !       1.39 eA-3
C187 0.502 0.747 0.909 !       1.38 eA-3
Q188 0.506 0.184 0.515 !       1.38 eA-3
Q189 0.343 0.186 0.643 !       1.38 eA-3
C190 0.332 0.392 0.748 !       1.37 eA-3
C191 0.496 0.296 0.736 !       1.37 eA-3
Q192 0.723 0.495 0.142 !       1.36 eA-3
C193 0.155 0.389 0.717 !       1.35 eA-3
Q194 0.971 0.420 0.358 !       1.35 eA-3
C195 0.688 0.605 0.265 !       1.35 eA-3
Q196 0.751 0.814 0.047 !       1.34 eA-3
Q197 1.008 0.346 0.606 !       1.34 eA-3
C198 0.541 0.262 0.594 !       1.34 eA-3
Q199 0.098 0.123 0.502 !       1.33 eA-3
;
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Flack x determined using 2168 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.049(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         9426
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.1151
_refine_ls_R_factor_gt           0.0684
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0595P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1458
_reflns_Friedel_coverage         0.996
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                6022
_reflns_number_total             9426
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00689_si_002.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               4089072
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2014/6
_shelx_res_checksum              39297
_shelx_hkl_checksum              6769