Polymerization of phenylacetylenes by binuclear rhodium catalysts with different para-binucleating phenoxyiminato linkages
Wu, Xiaolu; Zhang, Pengfei; Yang, Zhi; Zhang, Shaowen; Liu, Hao; Chi, Weijie; Li, Xiaofang; Dong, Yuping; Qiu, Nannan; Yan, Li; Polymer Chemistry 10 (2019) 4163–; doi:10.1039/C9PY00594C

data_1551938
_publ_section_title
;
 Polymerization of phenylacetylenes by binuclear rhodium catalysts with
 different para-binucleating phenoxyiminato linkages
;
_journal_issue                   30
_journal_name_full               'Polymer Chemistry'
_journal_page_first              4163
_journal_paper_doi               10.1039/C9PY00594C
_journal_volume                  10
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C44 H42 N2 O2 Rh2, C H Cl3'
_chemical_formula_sum            'C45 H43 Cl3 N2 O2 Rh2'
_chemical_formula_weight         955.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-12-13
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2017-01-17 deposited with the CCDC.    2019-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.88(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   19.411(4)
_cell_length_b                   10.281(2)
_cell_length_c                   9.972(2)
_cell_measurement_reflns_used    3285
_cell_measurement_temperature    153.1500
_cell_measurement_theta_max      27.4739
_cell_measurement_theta_min      2.1061
_cell_volume                     1982.8(7)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
????
;
_diffrn_ambient_temperature      153.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 98.8000
_diffrn_measured_fraction_theta_max 27.4739
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 44.7485
              2theta: -20.2210
scan:
    Number of images: 240
               Slice: -110.0000 - 10.0000
         Image width: 0.5000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 44.7485
              2theta: -20.2210
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       dtprofit.ref
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0279
_diffrn_orient_matrix_UB_12      0.0321
_diffrn_orient_matrix_UB_13      -0.0294
_diffrn_orient_matrix_UB_21      0.0029
_diffrn_orient_matrix_UB_22      -0.0669
_diffrn_orient_matrix_UB_23      -0.0705
_diffrn_orient_matrix_UB_31      -0.0798
_diffrn_orient_matrix_UB_32      0.0428
_diffrn_orient_matrix_UB_33      -0.0439
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710747
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_av_unetI/netI     0.0842
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5561
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.05
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           90.0000
_diffrn_source_power             4.5000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    1.076
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5593
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.027
_refine_diff_density_min         -1.898
_refine_diff_density_rms         0.431
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(11)
_refine_ls_extinction_coef       0.0047(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         3204
_refine_ls_number_restraints     337
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0818
_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^)+(0.1770P)^2^+8.6680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2208
_refine_ls_wR_factor_ref         0.2663
_reflns_number_gt                2880
_reflns_number_total             3204
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9py00594c2.cif
_cod_data_source_block           bwn16285
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 1551934--1551938.cif.
;
_cod_original_formula_sum        C45H43Cl3N2O2Rh2
_cod_database_code               1551938
_diffrn_number_total             2377
_olex2_refinement_description
;
1. 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
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.02
3. Others
 Fixed Sof: C23(0.5) H23(0.5)
4.a Riding coordinates:
 C23(H23)
4.b Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C16(H16)
4.c Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B)
4.d Aromatic/amide H refined with riding coordinates:
 C9(H9), C11(H11), C12(H12), C14(H14), C18(H18), C19(H19), C20(H20), C21(H21),
 C22(H22)
4.e Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C)
;
_olex2_submission_special_instructions 'No special instructions were received'