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_7702988
_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 Al0.5 N2 P), Cl4 Ga'
_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                   12.6047(3)
_cell_length_b                   12.6047(3)
_cell_length_c                   58.597(2)
_cell_measurement_reflns_used    17239
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.63
_cell_measurement_theta_min      1.39
_cell_volume                     8062.5(4)
_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  'Olex2 (Dolomanov et al., 2009)'
_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 0.963
_diffrn_measured_fraction_theta_max 0.963
_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  0.0597
_diffrn_reflns_av_unetI/netI     0.1061
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       71
_diffrn_reflns_limit_l_min       -70
_diffrn_reflns_number            20530
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.553
_diffrn_reflns_theta_max         25.553
_diffrn_reflns_theta_min         1.866
_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    0.827
_exptl_absorpt_correction_T_max  0.8516
_exptl_absorpt_correction_T_min  0.6424
_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    1.341
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3372
_exptl_crystal_size_max          0.523
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.178
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;
 Flack x determined using 2034 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.024(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.942
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         9628
_refine_ls_number_restraints     186
_refine_ls_restrained_S_all      0.935
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0332P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0767
_refine_ls_wR_factor_ref         0.0813
_reflns_Friedel_coverage         0.734
_reflns_Friedel_fraction_full    0.941
_reflns_Friedel_fraction_max     0.941
_reflns_number_gt                6842
_reflns_number_total             9628
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04082j2.cif
_cod_data_source_block           bg312
_cod_depositor_comments
'Adding full bibliography for 7702984--7702988.cif.'
_cod_original_cell_volume        8062.5(5)
_cod_database_code               7702988
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.867
_shelx_estimated_absorpt_t_min   0.671
_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 bond restraints
 C43, C44, C45, C46, C47, C48, C49
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C29, C30B, C31B, C32B, C33B, C34B, C35B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C29 \\sim C30B \\sim C31B \\sim C32B \\sim C33B \\sim C34B \\sim C35B: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 C30A, C31A, C32A, C33A, C34A, C35A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C30B, C31B, C32B, C33B, C34B, C35B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H29A(0.6) H29(0.4) C30A(0.4) C31A(0.4) H31A(0.4) C32A(0.4)
 H32A(0.4) C33A(0.4) H33A(0.4) C34A(0.4) H34A(0.4) C35A(0.4) H35A(0.4)
 C30B(0.6) C31B(0.6) H31B(0.6) C32B(0.6) H32B(0.6) C33B(0.6) H33B(0.6)
 C34B(0.6) H34B(0.6) C35B(0.6) H35B(0.6)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C15(H15), C29(H29A), C29(H29), C43(H43)
6.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), C38(H38), C39(H39), C40(H40),
 C41(H41), C42(H42), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49), C52(H52),
  C53(H53), C54(H54), C55(H55), C56(H56), C31A(H31A), C32A(H32A), C33A(H33A),
 C34A(H34A), C35A(H35A), C31B(H31B), C32B(H32B), C33B(H33B), C34B(H34B),
 C35B(H35B)
6.c Fitted hexagon refined as free rotating group:
 C30A(C31A,C32A,C33A,C34A,C35A), C30B(C31B,C32B,C33B,C34B,C35B)
6.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              51419
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'