Neutral and cationic enantiopure group 13 iminophosphonamide complexes.
Goswami, Bhupendra; Yadav, Ravi; Schoo, Christoph; Roesky, Peter W.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 675–681; doi:10.1039/c9dt04082j

data_7702987
_publ_section_title
;
 Neutral and cationic enantiopure group 13 iminophosphonamide complexes.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              675
_journal_page_last               681
_journal_paper_doi               10.1039/c9dt04082j
_journal_volume                  49
_journal_year                    2020
_chemical_absolute_configuration syn
_chemical_formula_moiety         '2(C28 H28 Ga0.5 N2 P), Al Cl4'
_chemical_formula_sum            'C56 H56 Al Cl4 Ga N4 P2'
_chemical_formula_weight         1085.48
_space_group_crystal_system      trigonal
_space_group_IT_number           152
_space_group_name_Hall           'P 31 2"'
_space_group_name_H-M_alt        'P 31 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-25
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_audit_update_record
;
2019-10-17 deposited with the CCDC.	2019-12-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   12.6494(2)
_cell_length_b                   12.6494(2)
_cell_length_c                   58.6453(12)
_cell_measurement_reflns_used    18268
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.56
_cell_measurement_theta_min      1.86
_cell_volume                     8126.5(2)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_data_reduction
;
X-Area Integrate 1.71.0.0 (STOE, 2016)
X-Area X-Red32 1.63.2.0 (STOE, 2017) 
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.77, Darmstadt 2016
;
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1149
_diffrn_reflns_av_unetI/netI     0.1168
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       71
_diffrn_reflns_limit_l_min       -70
_diffrn_reflns_number            28278
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.606
_diffrn_reflns_theta_max         25.606
_diffrn_reflns_theta_min         1.859
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           0.000
_diffrn_source_power             0.000
_diffrn_source_voltage           0
_exptl_absorpt_coefficient_mu    0.821
_exptl_absorpt_correction_T_max  0.9353
_exptl_absorpt_correction_T_min  0.6003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'STOE XRED, XSHAPE & LANA'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_description       prism
_exptl_crystal_F_000             3372
_exptl_crystal_size_max          0.258
_exptl_crystal_size_mid          0.158
_exptl_crystal_size_min          0.081
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Flack x determined using 1855 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.024(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         10102
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1150
_refine_ls_R_factor_gt           0.0654
_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^)+(0.0370P)^2^+9.6329P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1306
_reflns_Friedel_coverage         0.739
_reflns_Friedel_fraction_full    0.978
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                6721
_reflns_number_total             10102
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04082j2.cif
_cod_data_source_block           bg318
_cod_depositor_comments
'Adding full bibliography for 7702984--7702988.cif.'
_cod_original_cell_volume        8126.5(3)
_cod_database_code               7702987
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.936
_shelx_estimated_absorpt_t_min   0.816
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 C44B, C49B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C47A, C48A, C49A, C44A, C45A, C46A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C44B, C45B, C46B, C47B, C48B, C49B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: H43A(0.5) H43(0.5) C44B(0.5) C49B(0.5) H49B(0.5) C48B(0.5)
 H48B(0.5) C47B(0.5) H47B(0.5) C46B(0.5) H46B(0.5) C45B(0.5) H45B(0.5)
 C47A(0.5) H47A(0.5) C46A(0.5) H46A(0.5) C45A(0.5) H45A(0.5) C44A(0.5)
 C49A(0.5) H49A(0.5) C48A(0.5) H48A(0.5)
4.a Ternary CH refined with riding coordinates:
 C1(H1), C15(H15), C29(H29), C43(H43A), C43(H43)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C24(H24),
  C25(H25), C26(H26), C27(H27), C28(H28), C31(H31), C32(H32), C33(H33),
 C34(H34), C35(H35), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42),
 C49B(H49B), C48B(H48B), C47B(H47B), C46B(H46B), C45B(H45B), C52(H52), C53(H53),
  C54(H54), C55(H55), C56(H56), C47A(H47A), C46A(H46A), C45A(H45A), C49A(H49A),
 C48A(H48A)
4.c Fitted hexagon refined as free rotating group:
 C44B(C49B,C48B,C47B,C46B,C45B), C47A(C46A,C45A,C44A,C49A,C48A)
4.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C22(H22A,H22B,H22C), C36(H36A,H36B,H36C), C50(H50A,H50B,H50C)
;
_shelx_res_checksum              9954
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'