Tandem double hydrophosphination of α,β,γ,δ-unsaturated-1,3-indandiones: diphosphine synthesis, mechanistic investigations and coordination chemistry.
Balázs, László B; Khalikuzzaman, Jasmina B.; Csókás, Dániel; Li, Yongxin; Pullarkat, Sumod A.; Leung, Pak-Hing; Chemical Communications  (2019) –; doi:10.1039/C9CC05384K

data_7124012
_publ_section_title
;
 Tandem double hydrophosphination of
 \a,\b,\g,\d-unsaturated-1,3-indandiones: diphosphine synthesis,
 mechanistic investigations and coordination chemistry.
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC05384K
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_sum            'C62 H61 Cl N2 O2 P2 Pd2'
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_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_update_record
;
2019-07-03 deposited with the CCDC.    2019-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4070(9)
_cell_length_b                   14.9513(11)
_cell_length_c                   31.156(3)
_cell_measurement_reflns_used    6404
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      30.0411
_cell_measurement_theta_min      2.2457
_cell_volume                     5313.6(8)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'APEX3 (Bruker AXS Inc., 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    'XP (Bruker AXS Inc., 2018)'
_computing_publication_material  'APEX3 (Bruker AXS Inc., 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'XT, VERSION 2014/5'
_diffrn_ambient_temperature      100.(2)
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_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Photon II CPADs detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Multilayer Mirror'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_unetI/netI     0.1168
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
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_diffrn_reflns_limit_k_min       -22
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_diffrn_reflns_theta_max         31.61
_diffrn_reflns_theta_min         2.21
_diffrn_source                   'Incoatec microfocus source'
_diffrn_source_type              'Bruker D8 Quest'
_exptl_absorpt_coefficient_mu    0.834
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.55
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
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_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.100
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_refine_diff_density_max         2.531
_refine_diff_density_min         -1.631
_refine_ls_abs_structure_details
;

Flack x determined using 3707 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.028(19)
_refine_ls_extinction_method     none
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_refine_ls_number_reflns         17602
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_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.1164
_refine_ls_R_factor_gt           0.0780
_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^)+(0.0150P)^2^+27.7463P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1411
_refine_ls_wR_factor_ref         0.1560
_reflns_number_gt                12456
_reflns_number_total             17602
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc05384k2.cif
_cod_data_source_block           leung1116m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        5313.6(7)
_cod_database_code               7124012
_shelx_res_checksum              1356