Synthesis of an expanded pincer ligand and its bimetallic coinage metal complexes.
Delaney, Andie R.; Yu, Li-Juan; Coote, Michelle L.; Colebatch, Annie L.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 11909–11917; doi:10.1039/d1dt01741a

data_7707975
_publ_section_title
;
 Synthesis of an expanded pincer ligand and its bimetallic coinage metal
 complexes.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11909
_journal_page_last               11917
_journal_paper_doi               10.1039/d1dt01741a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C24 H40 Cu2 I2 N2 O2 P2'
_chemical_formula_sum            'C24 H40 Cu2 I2 N2 O2 P2'
_chemical_formula_weight         831.40
_chemical_name_systematic        tBuPONNOPCu2I2
_space_group_crystal_system      tetragonal
_space_group_IT_number           113
_space_group_name_Hall           'P -4 2ab'
_space_group_name_H-M_alt        'P -4 21 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-27 deposited with the CCDC.	2021-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.19560(10)
_cell_length_b                   13.19560(10)
_cell_length_c                   8.87860(10)
_cell_measurement_reflns_used    13601
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.6520
_cell_measurement_theta_min      5.9840
_cell_volume                     1545.98(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -85.00 -48.00   1.00    1.00    --  -37.08 125.00 -30.00   37
  2  \w    -31.00  -6.00   1.00    1.00    --  -37.08 125.00 -30.00   25
  3  \w     16.00  53.00   1.00    1.00    --   37.08 -57.00-180.00   37
  4  \w     21.00 104.00   1.00    1.00    --   37.08  57.00-180.00   83
  5  \w     25.00  53.00   1.00    1.00    --   37.08 -57.00 120.00   28
  6  \w     37.00  84.00   1.00    1.00    --   37.08-125.00 150.00   47
  7  \w    -26.00  13.00   1.00    1.00    --   37.08 -57.00-180.00   39
  8  \w     28.00  61.00   1.00    1.00    --   37.08-125.00-180.00   33
  9  \w    -34.00  66.00   1.00    1.00    --   37.08 -19.00-150.00  100
 10  \w     49.00  88.00   1.00    1.00    --   37.08  57.00 120.00   39
 11  \w     48.00  74.00   1.00    1.00    --   37.08  38.00 -90.00   26
 12  \w    -21.00  62.00   1.00    1.00    --   37.08 -77.00 -30.00   83
 13  \w     24.00  51.00   1.00    1.00    --   37.08  57.00   0.00   27
 14  \w     37.00  76.00   1.00    1.00    --   37.08 -99.00-120.00   39
 15  \w     62.00  89.00   1.00    1.00    --   37.08  38.00   0.00   27
 16  \w     30.00  55.00   1.00    1.00    --   37.08  38.00   0.00   25
 17  \w     22.00  98.00   1.00    1.00    --   37.08  38.00  90.00   76
 18  \w     42.00  68.00   1.00    1.00    --  111.00-111.00 150.00   26
 19  \w     90.00 129.00   1.00    1.00    --  111.00 -38.00-180.00   39
 20  \w    112.00 159.00   1.00    1.00    --  111.00 111.00 -90.00   47
 21  \w     60.00 105.00   1.00    1.00    --  111.00 -38.00  30.00   45
 22  \w     45.00  95.00   1.00    1.00    --  111.00 -64.00 -60.00   50
 23  \w     92.00 172.00   1.00    1.00    --  111.00  38.00  30.00   80
 24  \w    111.00 137.00   1.00    1.00    --  111.00 -77.00  90.00   26
 25  \w     48.00 100.00   1.00    1.00    --  111.00 -12.00 -90.00   52
 26  \w     93.00 156.00   1.00    1.00    --  111.00  25.00-180.00   63
 27  \w     48.00  75.00   1.00    1.00    --  111.00 -92.00  90.00   27
 28  \w     81.00 106.00   1.00    1.00    --  111.00 -92.00 150.00   25
 29  \w    121.00 148.00   1.00    1.00    --  111.00  50.00 150.00   27
 30  \w     83.00 109.00   1.00    1.00    --  111.00-111.00 150.00   26
 31  \w    125.00 152.00   1.00    1.00    --  111.00  25.00-150.00   27
 32  \w    102.00 143.00   1.00    1.00    --  111.00 -87.00 -45.76   41
 33  \w     83.00 109.00   1.00    1.00    --  111.00-111.00-150.00   26
 34  \w     61.00  87.00   1.00    1.00    --  111.00 178.00  30.00   26
 35  \w     48.00  75.00   1.00    1.00    --  111.00-111.00-150.00   27
 36  \w     94.00 151.00   1.00    1.00    --  111.00  50.00  90.00   57
 37  \w     69.00 105.00   1.00    1.00    --  111.00-111.00 120.00   36
 38  \w    112.00 145.00   1.00    1.00    --  111.00 -17.00 177.83   33
 39  \w    141.00 166.00   1.00    1.00    --  111.00 111.00  30.00   25
 40  \w    110.00 137.00   1.00    1.00    --  111.00 111.00  30.00   27
 41  \w     43.00 130.00   1.00    1.00    --  111.00 -38.00 120.00   87
 42  \w    123.00 168.00   1.00    1.00    --  111.00 111.00-180.00   45
 43  \w     69.00 109.00   1.00    1.00    --  111.00-111.00  60.00   40
 44  \w     68.00 108.00   1.00    1.00    --  111.00-111.00 -30.00   40
 45  \w     81.00 109.00   1.00    1.00    --  111.00-111.00 -90.00   28
 46  \w    131.00 161.00   1.00    1.00    --  111.00  77.00 -30.00   30
 47  \w     94.00 131.00   1.00    1.00    --  111.00 -64.00  60.00   37
 48  \w    100.00 127.00   1.00    1.00    --  111.00  64.00-150.00   27
 49  \w    131.00 169.00   1.00    1.00    --  111.00  64.00-150.00   38
 50  \w    106.00 131.00   1.00    1.00    --  111.00 -64.00 -90.00   25
 51  \w     47.00  89.00   1.00    1.00    --  111.00 -38.00 -90.00   42
 52  \w    102.00 129.00   1.00    1.00    --  111.00 -38.00 -90.00   27
 53  \w     71.00  98.00   1.00    1.00    --  111.00-111.00-120.00   27
 54  \w     93.00 134.00   1.00    1.00    --  111.00 -77.00 150.00   41
 55  \w     60.00 109.00   1.00    1.00    --  111.00-111.00 -60.00   49
 56  \w     60.00 100.00   1.00    1.00    --  111.00 -92.00 120.00   40
 57  \w     46.00 106.00   1.00    1.00    --  111.00 -17.00 177.83   60
 58  \w     82.00 107.00   1.00    1.00    --  111.00-111.00   0.00   25
 59  \w     44.00  70.00   1.00    1.00    --  111.00 -87.00 -45.76   26
 60  \w     81.00 106.00   1.00    1.00    --  111.00 -50.00  90.00   25
 61  \w     68.00  93.00   1.00    1.00    --  111.00 -50.00 150.00   25
 62  \w     92.00 137.00   1.00    1.00    --  111.00 -82.00-147.94   45
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0624139000
_diffrn_orient_matrix_UB_12      0.0978099000
_diffrn_orient_matrix_UB_13      0.0191494000
_diffrn_orient_matrix_UB_21      0.0209900000
_diffrn_orient_matrix_UB_22      0.0017014000
_diffrn_orient_matrix_UB_23      -0.1706370000
_diffrn_orient_matrix_UB_31      -0.0964070000
_diffrn_orient_matrix_UB_32      0.0637594000
_diffrn_orient_matrix_UB_33      -0.0247377000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0903
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            17949
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.821
_diffrn_reflns_theta_min         4.739
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.530
_exptl_absorpt_correction_T_max  0.447
_exptl_absorpt_correction_T_min  0.009
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.36a (Rigaku Oxford Diffraction, 2018)
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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.786
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichloromethane/hexane'
_exptl_crystal_size_max          0.596
_exptl_crystal_size_mid          0.199
_exptl_crystal_size_min          0.146
_refine_diff_density_max         1.689
_refine_diff_density_min         -1.728
_refine_diff_density_rms         0.175
_refine_ls_abs_structure_details
;
 Flack x determined using 695 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     96
_refine_ls_number_reflns         1667
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0778P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.0988
_reflns_Friedel_coverage         0.733
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                1662
_reflns_number_total             1667
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01741a2.cif
_cod_data_source_block           Cu2I2tBuPONNOP
_cod_depositor_comments
'Adding full bibliography for 7707971--7707976.cif.'
_cod_original_cell_volume        1545.98(3)
_cod_database_code               7707975
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C24H40Cu2I2N2O2P2
_reflns_odcompleteness_completeness 99.18
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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:
 C4(H4), C3(H3)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              54451
_shelx_hkl_checksum              52688
_ins_header
;
TITL AD109_correctedformula in P-42(1)m 
REM P-42(1)m (#113 in standard setting)
CELL 1.54184  13.195624  13.195624   8.878621  90.0000  90.0000  90.0000
ZERR    2.00   0.000099   0.000099   0.000130   0.0000   0.0000   0.0000
LATT -1
SYMM -x,-y, z 
SYMM  y,-x,-z 
SYMM -y, x,-z 
SYMM -x+1/2, y+1/2,-z 
SYMM  x+1/2,-y+1/2,-z 
SYMM -y+1/2,-x+1/2, z 
SYMM  y+1/2, x+1/2, z 
SFAC C H N O P Cu I
UNIT 48.00 80.00 4.00 4.00 4.00 4.00 4.00
TREF
HKLF 4
END
;
_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 3.442
_oxdiff_exptl_absorpt_empirical_full_min 0.252