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_7703497
_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 Cl2 Ir O3 P2'
_chemical_formula_sum            'C29 H49 Cl2 Ir O3 P2'
_chemical_formula_weight         770.72
_chemical_melting_point          ?
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-04-17
_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            8
_cell_length_a                   12.4393(2)
_cell_length_b                   13.2278(2)
_cell_length_c                   39.2327(7)
_cell_measurement_reflns_used    25050
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.9570
_cell_measurement_theta_min      3.5210
_cell_volume                     6455.53(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (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      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    -20.00  65.00   1.00   27.50    --   24.25 -99.00  60.00   85
  2  \w     -4.00  97.00   1.00   27.50    --   24.25  57.00 -90.00  101
  3  \w      0.00  99.00   1.00   27.50    --   24.25  37.00-150.00   99
  4  \w    -99.00 -14.00   1.00   27.50    --  -23.31 -77.00  90.00   85
  5  \w    -29.00  52.00   1.00   27.50    --   24.25 -57.00 -90.00   81
  6  \w    -48.00  52.00   1.00   27.50    --   24.25 -57.00 120.00  100
;
_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      -0.0563343000
_diffrn_orient_matrix_UB_12      0.0079041000
_diffrn_orient_matrix_UB_13      -0.0007798000
_diffrn_orient_matrix_UB_21      -0.0024181000
_diffrn_orient_matrix_UB_22      0.0003756000
_diffrn_orient_matrix_UB_23      0.0180727000
_diffrn_orient_matrix_UB_31      0.0084305000
_diffrn_orient_matrix_UB_32      0.0530329000
_diffrn_orient_matrix_UB_33      -0.0000113000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0731
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            68739
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        70.070
_diffrn_reflns_theta_max         70.070
_diffrn_reflns_theta_min         6.789
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    10.681
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.653
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (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    1.586
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3104
_exptl_crystal_recrystallization_method 'Crystals grown from hexane at 293 K'
_exptl_crystal_size_max          0.168
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.024
_refine_diff_density_max         2.321
_refine_diff_density_min         -3.870
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.445
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         6116
_refine_ls_number_restraints     258
_refine_ls_restrained_S_all      1.417
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0677
_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^)+87.5375P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1237
_refine_ls_wR_factor_ref         0.1260
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5406
_reflns_number_total             6116
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04835a3.cif
_cod_data_source_block           0327abc17s
_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_original_cell_volume        6455.6(2)
_cod_database_code               7703497
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C219-C118 \\sim C119-C118 \\sim C220-C219 \\sim C120-C119 \\sim C220-C121
\\sim C121-C120 \\sim C122-
 C121 \\sim C222-C121 \\sim C123-C122 \\sim C223-C222 \\sim C223-C124 \\sim
C124-C123
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C118 \\sim C119 \\sim C120 \\sim C121 \\sim C122 \\sim C123 \\sim C124 \\sim
C219 \\sim C220 \\sim C222 \\sim C223: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C118) \\sim Ueq, Uanis(C121) \\sim Ueq, Uanis(C124) \\sim Ueq,
Uanis(C119) \\sim Ueq, Uanis(C120) \\sim Ueq, Uanis(C122) \\sim Ueq,
Uanis(C123) \\sim Ueq, Uanis(C220) \\sim Ueq, Uanis(C222) \\sim Ueq,
Uanis(C219) \\sim Ueq, Uanis(C223) \\sim Ueq: with sigma of 0.007 and sigma for
terminal atoms of 0.014
4. Others
 Sof(H11W)=Sof(H11X)=Sof(H12E)=Sof(H12F)=Sof(H12M)=Sof(H12N)=Sof(C219)=
 Sof(H21A)=Sof(H21B)=Sof(C220)=Sof(H22A)=Sof(H22B)=Sof(C222)=Sof(H22C)=
 Sof(H22D)=Sof(C223)=Sof(H22E)=Sof(H22F)=1-FVAR(1)
 Sof(H11U)=Sof(H11V)=Sof(C119)=Sof(H11Y)=Sof(H)=Sof(C120)=Sof(H12A)=Sof(H12B)=
 Sof(H12C)=Sof(H12D)=Sof(C122)=Sof(H12G)=Sof(H12H)=Sof(C123)=Sof(H12I)=
 Sof(H12J)=Sof(H12K)=Sof(H12L)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C117(H11S,H11T), C118(H11U,H11V), C118(H11W,H11X), C119(H11Y,H), C120(H12A,
 H12B), C121(H12C,H12D), C121(H12E,H12F), C122(H12G,H12H), C123(H12I,H12J),
 C124(H12K,H12L), C124(H12M,H12N), C125(H12O,H12P), C126(H12Q,H12R), C127(H12S,
 H12T), C128(H12U,H12V), C129(H12W,H12X), C130(H13A,H13B), C219(H21A,H21B),
 C220(H22A,H22B), C222(H22C,H22D), C223(H22E,H22F)
5.b Aromatic/amide H refined with riding coordinates:
 C103(H103), C104(H104), C105(H105)
5.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              43978
_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 1.800
_oxdiff_exptl_absorpt_empirical_full_min 0.561