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_7702984
_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 H57 Al N4 P2'
_chemical_formula_sum            'C56 H57 Al N4 P2'
_chemical_formula_weight         874.97
_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   difmap
_atom_sites_solution_primary     dual
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Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
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_audit_update_record
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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                   18.1730(2)
_cell_length_b                   14.6537(5)
_cell_length_c                   9.8443(6)
_cell_measurement_reflns_used    21387
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.42
_cell_measurement_theta_min      1.79
_cell_volume                     2621.55(19)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
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X-Area Integrate 1.71.0.0 (STOE, 2016)
X-Area X-Red32 1.63.2.0 (STOE, 2017) 
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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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)'
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_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
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_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0424
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            35079
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.546
_diffrn_reflns_theta_min         1.785
_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    0.138
_exptl_absorpt_correction_T_max  0.9776
_exptl_absorpt_correction_T_min  0.7996
_exptl_absorpt_correction_type   multi-scan
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_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.108
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.279
_exptl_crystal_size_mid          0.228
_exptl_crystal_size_min          0.188
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.183
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details
;
 Flack x determined using 2095 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.06(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         7327
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0522P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0862
_reflns_Friedel_coverage         0.786
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                5686
_reflns_number_total             7327
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04082j2.cif
_cod_data_source_block           bg086
_cod_depositor_comments
'Adding full bibliography for 7702984--7702988.cif.'
_cod_database_code               7702984
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.963
_olex2_refinement_description
;
1. Rigid bond restraints
 C3, C2, C7, C6, C5, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              1195
_shelx_fab_checksum              74544
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'