Synthesis and group 9 complexes of macrocyclic PCP and POCOP pincer ligands.
Leforestier, Baptiste; Gyton, Matthew R.; Chaplin, Adrian B.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 2087–2101; doi:10.1039/c9dt04835a

data_7703495
_publ_section_title
;
 Synthesis and group 9 complexes of macrocyclic PCP and POCOP pincer
 ligands.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2087
_journal_page_last               2101
_journal_paper_doi               10.1039/c9dt04835a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C29 H49 Ir O3 P2'
_chemical_formula_sum            'C29 H49 Ir O3 P2'
_chemical_formula_weight         699.82
_chemical_melting_point          ?
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-10-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-18 deposited with the CCDC.	2020-01-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.8772(2)
_cell_length_b                   10.65296(8)
_cell_length_c                   13.56659(11)
_cell_measurement_reflns_used    18690
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.5080
_cell_measurement_theta_min      3.8720
_cell_volume                     3017.26(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_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      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3046
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -87.00  -6.00   1.00    1.00    --  -41.82 125.00 -90.00   81
  2  \w      6.00  83.00   1.00    1.00    --   41.82 -99.00   0.00   77
  3  \w     14.00 115.00   1.00    1.00    --   41.82  57.00-120.00  101
  4  \w     27.00  98.00   1.00    1.00    --   41.82-125.00  90.00   71
  5  \w     97.00 178.00   1.00    1.20    --  107.00 125.00 -90.00   81
  6  \w     97.00 178.00   1.00    1.20    --  107.00 125.00 -60.00   81
  7  \w     81.00 178.00   1.00    1.20    --  107.00  45.00 150.00   97
  8  \w    103.00 178.00   1.00    1.20    --  107.00  77.00  60.00   75
  9  \w     34.00 133.00   1.00    1.20    --  107.00 -45.00-120.00   99
 10  \w     35.00 136.00   1.00    1.20    --  107.00 -61.00-180.00  101
 11  \w   -116.00 -17.00   1.00    1.00    --  -41.82 -37.00 -90.00   99
 12  \w   -114.00 -14.00   1.00    1.00    --  -41.82 -57.00   0.00  100
 13  \w   -114.00 -14.00   1.00    1.00    --  -41.82 -57.00  90.00  100
 14  \w     78.00 178.00   1.00    1.20    --  107.00  61.00 -90.00  100
 15  \w     81.00 178.00   1.00    1.20    --  107.00  45.00   0.00   97
 16  \w     34.00 105.00   1.00    1.20    --  107.00-125.00  90.00   71
 17  \w    103.00 178.00   1.00    1.20    --  107.00  77.00-150.00   75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku Oxford Diffraction: 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      -0.0281467000
_diffrn_orient_matrix_UB_12      0.0079892000
_diffrn_orient_matrix_UB_13      0.1047461000
_diffrn_orient_matrix_UB_21      0.0154403000
_diffrn_orient_matrix_UB_22      -0.1398513000
_diffrn_orient_matrix_UB_23      0.0164077000
_diffrn_orient_matrix_UB_31      0.0664460000
_diffrn_orient_matrix_UB_32      0.0359143000
_diffrn_orient_matrix_UB_33      0.0406613000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25010
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        70.073
_diffrn_reflns_theta_max         70.073
_diffrn_reflns_theta_min         6.526
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.772
_exptl_absorpt_correction_T_max  0.848
_exptl_absorpt_correction_T_min  0.190
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.57a (Rigaku Oxford Diffraction, 2019)
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            'dark yellow'
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1416
_exptl_crystal_recrystallization_method 'Crystals grown from TMS at 293 K'
_exptl_crystal_size_max          0.304
_exptl_crystal_size_mid          0.224
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.234(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         5667
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0205
_refine_ls_R_factor_gt           0.0192
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+0.4746P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0464
_refine_ls_wR_factor_ref         0.0467
_reflns_Friedel_coverage         0.913
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                5575
_reflns_number_total             5667
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04835a3.cif
_cod_data_source_block           0554abc19s
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7703488--7703497.cif.
;
_cod_database_code               7703495
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.766(9)
 0.234(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C117(H11S,H11T), C118(H11U,H11V), C119(H11W,H11X), C120(H12A,H12B), C121(H12C,
 H12D), C122(H12E,H12F), C123(H12G,H12H), C124(H12I,H12J), C125(H12K,H12L),
 C126(H12M,H12N), C127(H12O,H12P), C128(H12Q,H12R), C129(H12S,H12T), C130(H13A,
 H13B)
3.b Aromatic/amide H refined with riding coordinates:
 C103(H103), C104(H104), C105(H105)
3.c Idealised Me refined as rotating group:
 C110(H11A,H11B,H11C), C111(H11D,H11E,H11F), C112(H11G,H11H,H11I), C114(H11J,
 H11K,H11L), C115(H11M,H11N,H11O), C116(H11P,H11Q,H11R)
;
_shelx_res_checksum              71555
_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 1.195
_oxdiff_exptl_absorpt_empirical_full_min 0.882