Isolation of a Heavier Cyclobutadiene Analogue: 2,4-Digerma-1,3-diphosphacyclobutadiene
Wu, Yile; Liu, Liu; Su, Jue; Zhu, Jun; Ji, Zhe; Zhao, Yufen; Organometallics 35 (2016) 1593–; doi:10.1021/acs.organomet.6b00187

data_4088570
_publ_section_title
;
 Isolation of a Heavier Cyclobutadiene Analogue:
 2,4-Digerma-1,3-diphosphacyclobutadiene
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              1593
_journal_paper_doi               10.1021/acs.organomet.6b00187
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C58 H82 Ge2 N4 P2'
_chemical_formula_sum            'C58 H82 Ge2 N4 P2'
_chemical_formula_weight         1042.40
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-04-20
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.063(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.224(4)
_cell_length_b                   14.667(3)
_cell_length_c                   16.439(3)
_cell_measurement_reflns_used    6291
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.06
_cell_measurement_theta_min      2.48
_cell_volume                     5358.4(18)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      173(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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20768
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.66
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.222
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2208
_refine_diff_density_max         0.986
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         5271
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0702P)^2^+0.2506P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1165
_reflns_number_gt                4477
_reflns_number_total             5271
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00187_si_002.cif
_cod_data_source_block           3
_cod_original_cell_volume        5358.4(17)
_cod_database_code               4088570
_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:
 C25(H25), C28(H28), C13(H13), C16(H16)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C21(H21), C20(H20), C10(H10), C22(H22), C8(H8), C9(H9)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C17(H17A,H17B,H17C), C26(H26A,H26B,H26C), C5(H5A,H5B,H5C),
 C24(H24A,H24B,H24C), C12(H12A,H12B,H12C), C15(H15A,H15B,H15C), C27(H27A,H27B,
 H27C), C14(H14A,H14B,H14C), C29(H29A,H29B,H29C)
;
_olex2_submission_special_instructions 'No special instructions were received'