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_7707971
_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 Cl2 Cu2 N2 O2 P2'
_chemical_formula_sum            'C24 H40 Cl2 Cu2 N2 O2 P2'
_chemical_formula_weight         648.50
_chemical_name_systematic        tBuPONNOPCu2Cl2
_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             2021-07-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-26 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                   13.1203(3)
_cell_length_b                   13.1203(3)
_cell_length_c                   8.6767(4)
_cell_measurement_reflns_used    9875
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      31.4830
_cell_measurement_theta_min      3.8200
_cell_volume                     1493.63(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL n/a (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1872
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.944
_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    -12.00  15.00   1.00    1.75    --  -17.84 -77.00 -90.00   27
  2  \w    -50.00  40.00   1.00    1.75    --  -17.84  77.00 -60.00   90
  3  \w    -94.00 -21.00   1.00    1.75    --  -17.84 154.00 160.88   73
  4  \w    -93.00 -33.00   1.00    1.75    --  -17.84 153.00  68.11   60
  5  \w     -6.00  39.00   1.00    1.75    --   18.00  77.00 -60.00   45
  6  \w    -38.00  51.00   1.00    1.75    --   18.00 -77.00  60.00   89
  7  \w    -21.00  33.00   1.00    1.75    --   18.00  19.00  30.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0047518000
_diffrn_orient_matrix_UB_12      -0.0051300000
_diffrn_orient_matrix_UB_13      0.0810975000
_diffrn_orient_matrix_UB_21      -0.0477896000
_diffrn_orient_matrix_UB_22      -0.0243745000
_diffrn_orient_matrix_UB_23      -0.0099929000
_diffrn_orient_matrix_UB_31      0.0247895000
_diffrn_orient_matrix_UB_32      -0.0479655000
_diffrn_orient_matrix_UB_33      -0.0036399000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            20453
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.460
_diffrn_reflns_theta_min         3.472
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.733
_exptl_absorpt_correction_T_max  0.686
_exptl_absorpt_correction_T_min  0.326
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_description       block
_exptl_crystal_F_000             672
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichloromethane/hexane'
_exptl_crystal_size_max          0.889
_exptl_crystal_size_mid          0.428
_exptl_crystal_size_min          0.211
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 986 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.019(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     96
_refine_ls_number_reflns         2623
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0259
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0208P)^2^+0.3512P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0529
_refine_ls_wR_factor_ref         0.0554
_reflns_Friedel_coverage         0.739
_reflns_Friedel_fraction_full    0.984
_reflns_Friedel_fraction_max     0.901
_reflns_number_gt                2444
_reflns_number_total             2623
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01741a2.cif
_cod_data_source_block           tBuPONNOPCu2Cl2
_cod_depositor_comments
'Adding full bibliography for 7707971--7707976.cif.'
_cod_original_cell_volume        1493.63(10)
_cod_database_code               7707971
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C24H40N2O2P2Cu2Cl2
_shelx_estimated_absorpt_t_max   0.711
_shelx_estimated_absorpt_t_min   0.308
_reflns_odcompleteness_completeness 97.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.51
_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:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              94746
_shelx_hkl_checksum              60734
_ins_header
;
TITL AD257_scale1 in P-42(1)m 
REM P-42(1)m (#113 in standard setting)
CELL 0.71073  13.120323  13.120323   8.676683  90.0000  90.0000  90.0000
ZERR    2.00   0.000262   0.000262   0.000381   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 Cl Cu
UNIT 48.00 80.00 4.00 4.00 4.00 4.00 4.00
REM  CrysAlisPro recorded range (K): Min=150.0; max=150.1; aver:150.0
TEMP -123
SIZE 0.21 0.43 0.89
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 1.284
_oxdiff_exptl_absorpt_empirical_full_min 0.779