A Series of Isopropyl-Substituted Oligogermanes Pri3Ge(GePh2)nGePri3(n= 0–3) Featuring a Luminescent and Dichroic Pentagermane Pri3Ge(GePh2)3GePri3
Komanduri, Sangeetha P.; Shumaker, F. Alexander; Roewe, Kimberly D.; Wolf, Melanie; Uhlig, Frank; Moore, Curtis E.; Rheingold, Arnold L.; Weinert, Charles S.; Organometallics 35 (2016) 3240–; doi:10.1021/acs.organomet.6b00596

data_4086741
_publ_section_title
;
 A Series of Isopropyl-Substituted Oligogermanes Pri3Ge(GePh2)nGePri3(n=
 0--3) Featuring a Luminescent and Dichroic Pentagermane
 Pri3Ge(GePh2)3GePri3
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              3240
_journal_paper_doi               10.1021/acs.organomet.6b00596
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C54 H72 Ge5'
_chemical_formula_sum            'C54 H72 Ge5'
_chemical_formula_weight         1084.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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
_audit_creation_date             2016-04-25
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 106.184(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5478(11)
_cell_length_b                   12.6673(9)
_cell_length_c                   25.3940(18)
_cell_measurement_reflns_used    4389
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.34
_cell_measurement_theta_min      2.35
_cell_volume                     5112.0(6)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0711
_diffrn_reflns_av_unetI/netI     0.0905
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            28800
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         1.812
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.939
_exptl_absorpt_correction_T_max  0.123
_exptl_absorpt_correction_T_min  0.082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       plate
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.215
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         9333
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0525
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+11.1810P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.1044
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6557
_reflns_number_total             9333
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00596_si_002.cif
_cod_data_source_block           Compound_5
_cod_database_code               4086741
_shelx_estimated_absorpt_t_max   0.799
_shelx_estimated_absorpt_t_min   0.463
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2), C5(H5), C8(H8), C47(H47), C50(H50), C53(H53)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17), C18(H18),
 C19(H19), C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27),
  C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C35(H35), C36(H36),
 C37(H37), C38(H38), C39(H39), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C9(H9C,H9A,H9B), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C49(H49A,
 H49B,H49C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C)
;
_shelx_res_checksum              51866
_shelx_hkl_checksum              83246
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'