Group 14 Metal Terminal Phosphides: Correlating Structure with |JMP|
Eric C. Y. Tam; Nicola A. Maynard; David C. Apperley; J. David Smith; Martyn P. Coles; J. Robin Fulton; Inorganic Chemistry 51 (2012) 9403–9415; doi:10.1021/ic301208d

data_4330224
_publ_section_title
;
 Group 14 Metal Terminal Phosphides: Correlating Structure with |JMP|
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9403
_journal_page_last               9415
_journal_paper_doi               10.1021/ic301208d
_journal_volume                  51
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         '2(C41 H51 N2 P Sn), C7 H8'
_chemical_formula_sum            'C89 H110 N4 P2 Sn2'
_chemical_formula_weight         1535.14
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2010-07-08T08:39:04-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                69.422(1)
_cell_angle_beta                 84.810(1)
_cell_angle_gamma                74.862(1)
_cell_formula_units_Z            2
_cell_length_a                   12.6382(3)
_cell_length_b                   17.6553(4)
_cell_length_c                   19.5975(4)
_cell_measurement_reflns_used    32105
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.103
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     3951.74(16)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.721148E-1
_diffrn_orient_matrix_UB_12      0.00903
_diffrn_orient_matrix_UB_13      0.80035E-2
_diffrn_orient_matrix_UB_21      0.26824E-1
_diffrn_orient_matrix_UB_22      -0.64741E-2
_diffrn_orient_matrix_UB_23      -0.477166E-1
_diffrn_orient_matrix_UB_31      -0.282655E-1
_diffrn_orient_matrix_UB_32      0.614215E-1
_diffrn_orient_matrix_UB_33      -0.250964E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0894
_diffrn_reflns_av_unetI/netI     0.0901
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            66909
_diffrn_reflns_theta_full        27.09
_diffrn_reflns_theta_max         27.09
_diffrn_reflns_theta_min         3.4
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.719
_exptl_absorpt_correction_T_max  0.9641
_exptl_absorpt_correction_T_min  0.861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            'Dark orange'
_exptl_crystal_density_diffrn    1.29
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1604
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.809
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.11
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.03
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     828
_refine_ls_number_reflns         17382
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0994
_refine_ls_R_factor_gt           0.0553
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0546P)^2^+7.3332P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1391
_reflns_number_gt                11616
_reflns_number_total             17382
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301208d_si_001_2.cif
_cod_data_source_block           (2a)-jul510
_cod_original_cell_volume        3951.75(15)
_cod_database_code               4330224