Rhodium Complexes of a New Structurally Adaptive PNN-Pincer Type Ligand
Wanniarachchi, Sarath; Hewage, Jeewantha S.; Lindeman, Sergey V.; Gardinier, James R.; Organometallics 32 (2013) 2885–; doi:10.1021/om400151e

data_4080742
_publ_section_title
;
 Rhodium Complexes of a New Structurally Adaptive PNN-Pincer Type Ligand
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2885
_journal_paper_doi               10.1021/om400151e
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'I, C39 H44 N5 P Rh, 2(C H2 Cl2)'
_chemical_formula_sum            'C41 H48 Cl4 I N5 P Rh'
_chemical_formula_weight         1013.42
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-02-22
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_cell_angle_alpha                106.957(4)
_cell_angle_beta                 95.347(4)
_cell_angle_gamma                104.978(4)
_cell_formula_units_Z            2
_cell_length_a                   10.9887(5)
_cell_length_b                   13.7160(6)
_cell_length_c                   16.4225(7)
_cell_measurement_reflns_used    11276
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.5084
_cell_measurement_theta_min      3.4456
_cell_volume                     2248.79(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_details
;
  1 omega  -58.00   41.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6697  -57.0000   60.0000 99

  2 omega  -10.00   16.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6697  -37.0000  -60.0000 26

  3 omega  -10.00   76.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6697   37.0000 -120.0000 86

  4 omega  -58.00  -22.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6697  -37.0000  -60.0000 36

  5 omega  -16.00   28.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.8259  -99.0000  -60.0000 44

  6 omega  -97.00  -58.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.8259  178.0000 -180.0000 39

  7 omega  -22.00   90.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6697   77.0000   60.0000 112

  8 omega  -15.00   10.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6697   37.0000    0.0000 25

  9 omega   35.00  102.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6697  178.0000  -60.0000 67
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0330577000
_diffrn_orient_matrix_UB_12      0.0503675000
_diffrn_orient_matrix_UB_13      0.0314427000
_diffrn_orient_matrix_UB_21      -0.0593652000
_diffrn_orient_matrix_UB_22      0.0090571000
_diffrn_orient_matrix_UB_23      0.0072935000
_diffrn_orient_matrix_UB_31      -0.0011367000
_diffrn_orient_matrix_UB_32      -0.0243481000
_diffrn_orient_matrix_UB_33      0.0326680000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32086
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         3.45
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.373
_exptl_absorpt_correction_T_max  0.918
_exptl_absorpt_correction_T_min  0.687
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.3454
_exptl_crystal_size_mid          0.1786
_exptl_crystal_size_min          0.0626
_refine_diff_density_max         0.833
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         11112
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0235P)^2^+1.5137P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0630
_refine_ls_wR_factor_ref         0.0718
_reflns_number_gt                8986
_reflns_number_total             11112
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400151e_si_001.cif
_cod_data_source_block           cismer-6_2CH2Cl2
_cod_original_cell_volume        2248.81(17)
_cod_database_code               4080742
_chemical_oxdiff_formula         'C39 H44 N5 P Rh I (C H2 Cl2)2'
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H3(0.019) H5(0.023) H6(0.021) H7a(0.036) H7b(0.036) H7c(0.036)
 H11(0.018) H12(0.019) H13(0.02) H23(0.022) H24(0.023) H25(0.024) H26(0.024)
 H32(0.022) H33(0.027) H34(0.03) H35(0.03) H36(0.024) H42(0.021) H43(0.026)
 H44(0.028) H45(0.028) H46(0.024) H53a(0.053) H53b(0.053) H53c(0.053)
 H54a(0.034) H54b(0.034) H54c(0.034) H55a(0.054) H55b(0.054) H55c(0.054)
 H63a(0.043) H63b(0.043) H63c(0.043) H64a(0.048) H64b(0.048) H64c(0.048)
 H65a(0.039) H65b(0.039) H65c(0.039) H71a(0.027) H71b(0.027) H71c(0.027)
 H1Sa(0.039) H1Sb(0.039) H2Sa(0.034) H2Sb(0.034)
 Fixed X: H3(0.3531) H5(0.1731) H6(0.0959) H7a(0.2766) H7b(0.3) H7c(0.412)
 H11(0.2737) H12(0.4939) H13(0.4944) H23(-0.1096) H24(0.016) H25(0.1837)
 H26(0.2348) H32(-0.2942) H33(-0.4664) H34(-0.5069) H35(-0.3748) H36(-0.2012)
 H42(-0.0649) H43(-0.186) H44(-0.3778) H45(-0.4455) H46(-0.3272) H53a(0.0318)
 H53b(-0.0026) H53c(0.1067) H54a(0.0015) H54b(-0.1186) H54c(-0.1407) H55a(-
 0.2647) H55b(-0.2432) H55c(-0.1984) H63a(0.0115) H63b(-0.0452) H63c(0.0619)
 H64a(-0.0743) H64b(-0.1854) H64c(-0.2161) H65a(-0.2978) H65b(-0.2722) H65c(-
 0.2093) H71a(0.105) H71b(0.1732) H71c(0.2381) H1Sa(0.5372) H1Sb(0.4653)
 H2Sa(0.5408) H2Sb(0.4144)
 Fixed Y: H3(0.6666) H5(0.7514) H6(0.5755) H7a(0.8534) H7b(0.8903) H7c(0.8647)
 H11(0.2564) H12(0.3856) H13(0.5492) H23(0.1695) H24(0.2469) H25(0.406)
 H26(0.4821) H32(0.2259) H33(0.2962) H34(0.401) H35(0.4347) H36(0.3664)
 H42(0.0309) H43(-0.149) H44(-0.199) H45(-0.0706) H46(0.11) H53a(-0.0546) H53b(-
 0.0966) H53c(0.0139) H54a(0.1117) H54b(0.01) H54c(0.1151) H55a(0.0031) H55b(-
 0.0998) H55c(-0.0714) H63a(0.6052) H63b(0.6976) H63c(0.6669) H64a(0.6279)
 H64b(0.6616) H64c(0.5464) H65a(0.4534) H65b(0.566) H65c(0.4792) H71a(0.1543)
 H71b(0.1499) H71c(0.242) H1Sa(0.0307) H1Sb(0.1059) H2Sa(0.7466) H2Sb(0.6662)
 Fixed Z: H3(0.4121) H5(0.2302) H6(0.1427) H7a(0.4394) H7b(0.3568) H7c(0.4086)
 H11(0.3698) H12(0.4302) H13(0.3902) H23(-0.0757) H24(-0.1612) H25(-0.095)
 H26(0.0543) H32(0.2171) H33(0.2326) H34(0.1493) H35(0.051) H36(0.0362)
 H42(0.1277) H43(0.0684) H44(-0.0282) H45(-0.0714) H46(-0.0106) H53a(0.2736)
 H53b(0.3523) H53c(0.3701) H54a(0.476) H54b(0.4634) H54c(0.4492) H55a(0.2958)
 H55b(0.3149) H55c(0.2325) H63a(0.5014) H63b(0.4897) H63c(0.4364) H64a(0.2936)
 H64b(0.3406) H64c(0.269) H65a(0.3733) H65b(0.4474) H65c(0.4646) H71a(0.1073)
 H71b(0.196) H71c(0.1583) H1Sa(0.3571) H1Sb(0.4143) H2Sa(0.2655) H2Sb(0.1987)
;