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_7702985
_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         'C56 H56 Cl Ga N4 P2, 0.5(C4 H10 O)'
_chemical_formula_sum            'C58 H61 Cl Ga N4 O0.5 P2'
_chemical_formula_weight         989.21
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-24
_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                90
_cell_formula_units_Z            2
_cell_length_a                   18.4844(4)
_cell_length_b                   14.5247(8)
_cell_length_c                   10.2958(8)
_cell_measurement_reflns_used    9664
_cell_measurement_temperature    240
_cell_measurement_theta_max      26.78
_cell_measurement_theta_min      1.78
_cell_volume                     2764.2(3)
_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      240
_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 0.996
_diffrn_measurement_details
;
 144 frames, detector distance = 100 mm
;
_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  0.0639
_diffrn_reflns_av_unetI/netI     0.0943
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19503
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.493
_diffrn_reflns_theta_min         1.783
_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    0.644
_exptl_absorpt_correction_T_max  0.9419
_exptl_absorpt_correction_T_min  0.8095
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_description       plate
_exptl_crystal_F_000             1038
_exptl_crystal_size_max          0.429
_exptl_crystal_size_mid          0.284
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.685
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
;
 Flack x determined using 1151 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.012(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         7672
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.1388
_refine_ls_R_factor_gt           0.0635
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1082P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1590
_refine_ls_wR_factor_ref         0.1979
_reflns_Friedel_coverage         0.790
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                3984
_reflns_number_total             7672
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04082j2.cif
_cod_data_source_block           bg298
_cod_depositor_comments
'Adding full bibliography for 7702984--7702988.cif.'
_cod_original_formula_sum        'C58 H61 Cl Ga N4 O0.50 P2'
_cod_database_code               7702985
_shelx_shelxl_version_number     2018/3
_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. Restrained distances
 C32-C31 \\sim C29-C30
 with sigma of 0.02
 O1-C31 \\sim O1-C29
 with sigma of 0.02
 C32-O1 \\sim O1-C30
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O1 \\sim C29 \\sim C30 \\sim C31 \\sim C32: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 O1, C29, C30, C31, C32
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O1(0.25) C29(0.25) H29A(0.25) H29B(0.25) C30(0.25) H30C(0.25)
 H30A(0.25) H30B(0.25) C31(0.25) H31A(0.25) H31B(0.25) C32(0.25) H32A(0.25)
 H32B(0.25) H32C(0.25)
6.a Free rotating group:
 O1(C29,C30,C31,C32)
6.b Ternary CH refined with riding coordinates:
 C1(H1), C9(H9)
6.c Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C31(H31A,H31B)
6.d Me refined with riding coordinates:
 C30(H30C,H30A,H30B)
6.e Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24),
  C25(H25), C26(H26), C27(H27), C28(H28)
6.f Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C16(H16A,H16B,H16C), C32(H32A,H32B,H32C)
;
_shelx_res_checksum              17153
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'