Nitrogen-Phosphorus(III)-Chalcogen Macrocycles for the Synthesis of Polynuclear Silver(I) Sandwich Complexes.
Yogendra, Sivathmeehan; Hennersdorf, Felix; Weigand, Jan J.; Inorganic chemistry 56 (2017) 8698–8704; doi:10.1021/acs.inorgchem.7b00141

data_4349400
_publ_section_title
;
 Nitrogen-Phosphorus(III)-Chalcogen Macrocycles for the Synthesis of
 Polynuclear Silver(I) Sandwich Complexes.
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8698
_journal_page_last               8704
_journal_paper_doi               10.1021/acs.inorgchem.7b00141
_journal_volume                  56
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C13 H13 Cl2 N P2'
_chemical_formula_sum            'C13 H13 Cl2 N P2'
_chemical_formula_weight         316.08
_chemical_name_systematic
1-chloro-N-(chloro(phenyl)phosphanyl)-N-methyl-1-phenylphosphanamine
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-01-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.10824(7)
_cell_length_b                   13.14264(13)
_cell_length_c                   15.51520(17)
_cell_measurement_reflns_used    4604
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.7940
_cell_measurement_theta_min      4.4000
_cell_volume                     1449.45(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5700
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -33.00  30.00   0.50    0.50    --   41.48 -38.00 150.00  126
  2  \w     36.00 135.00   0.50    0.50    --  111.00 -30.00  90.00  198
  3  \w    132.00 177.00   0.50    0.50    --  111.00  77.00  30.00   90
  4  \w     58.00  84.00   0.50    0.50    --  111.00  15.00   0.00   52
  5  \w     25.00 155.00   0.50    0.50    --  111.00   0.00  60.00  260
  6  \w     41.00 138.00   0.50    0.50    --  111.00 -61.00  90.00  194
  7  \w     39.00 115.00   0.50    0.50    --  111.00-111.00 -90.00  152
  8  \w     41.00  84.00   0.50    0.50    --  111.00 -61.00  60.00   86
  9  \w   -116.00 -47.00   0.50    0.50    --  -41.48 -35.00-139.00  138
 10  \w   -114.00 -17.00   0.50    0.50    --  -41.48 -38.00  60.00  194
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0468601000
_diffrn_orient_matrix_UB_12      0.0055617000
_diffrn_orient_matrix_UB_13      -0.0968305000
_diffrn_orient_matrix_UB_21      0.0846311000
_diffrn_orient_matrix_UB_22      0.1078192000
_diffrn_orient_matrix_UB_23      -0.0042017000
_diffrn_orient_matrix_UB_31      0.1938976000
_diffrn_orient_matrix_UB_32      -0.0456459000
_diffrn_orient_matrix_UB_33      -0.0216693000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6697
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.112
_diffrn_reflns_theta_min         4.409
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.958
_exptl_absorpt_correction_T_max  0.535
_exptl_absorpt_correction_T_min  0.230
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       block
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.422
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.194
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Flack x determined using 1198 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.008(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         2991
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0246
_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^)+(0.0453P)^2^+0.0364P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0661
_reflns_Friedel_coverage         0.713
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                2939
_reflns_number_total             2991
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            MeN(PhPCl)2_file017_file017.cif
_cod_data_source_block           MeNPhPCl2
_cod_database_code               4349400
_chemical_oxdiff_formula         'C52 H52 Cl8 N4 P8 '
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_shelx_res_checksum              99259
_shelx_hkl_checksum              24114
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.450
_oxdiff_exptl_absorpt_empirical_full_min 0.677