Synthesis and structural characterisation of the first N-heterocyclic carbene ligand fused to a porphyrin.
Richeter, Sébastien; Hadj-Aïssa, Aurélie; Taffin, Céline; van der Lee, Arie; Leclercq, Dominique; Chemical communications (Cambridge, England)  (2007) 2148–2150; doi:10.1039/b704681b

data_7101932
_publ_section_title
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 Synthesis and structural characterisation of the first N-heterocyclic
 carbene ligand fused to a porphyrin.
;
_journal_issue                   21
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2148
_journal_page_last               2150
_journal_paper_doi               10.1039/b704681b
_journal_year                    2007
_chemical_formula_moiety         'C126 H128 I2 N12 Ni2 Pd, 4(C H Cl3)'
_chemical_formula_sum            'C130 H132 Cl12 I2 N12 Ni2 Pd'
_chemical_formula_weight         2765.48
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             07-03-21
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 103.730(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.1838(7)
_cell_length_b                   9.9174(4)
_cell_length_c                   31.4826(13)
_cell_measurement_reflns_used    7597
_cell_measurement_temperature    175
_cell_measurement_theta_max      32.4001
_cell_measurement_theta_min      2.5994
_cell_volume                     6728.4(5)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_collection
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CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2006)'
_diffrn_ambient_temperature      175
_diffrn_detector_area_resol_mean 8.4205
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.765
_diffrn_measurement_details
;
1 omega -54.00 61.00 1.0000 28.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 30.0000 -79.0000 0.0000 0.0000 0.0000 115

2 omega -54.00 61.00 1.0000 28.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 30.0000 -79.0000 90.0000 0.0000 0.0000 115

3 omega -54.00 61.00 1.0000 28.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 30.0000 -79.0000 180.0000 0.0000 0.0000 115

4 omega -54.00 61.00 1.0000 28.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 30.0000 -79.0000 270.0000 0.0000 0.0000 115

5 omega -50.00 10.00 1.0000 28.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -25.0000 -80.0000 100.0000 0.0000 0.0000 60

6 omega -116.00 71.00 1.0000 28.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -25.0000 -10.0000 180.0000 0.0000 0.0000 187

7 omega -50.00 12.00 1.0000 28.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -25.0000 -80.0000 0.0000 0.0000 0.0000 62
;
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_method       \w
_diffrn_orient_matrix_UB_11      -0.0020593581
_diffrn_orient_matrix_UB_12      0.0669046190
_diffrn_orient_matrix_UB_13      -0.0079646180
_diffrn_orient_matrix_UB_21      0.0190434265
_diffrn_orient_matrix_UB_22      0.0221160275
_diffrn_orient_matrix_UB_23      0.0201177432
_diffrn_orient_matrix_UB_31      0.0266433617
_diffrn_orient_matrix_UB_32      -0.0106853254
_diffrn_orient_matrix_UB_33      -0.0082136828
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.166
_diffrn_reflns_av_sigmaI/netI    0.3075
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            18567
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         32.480
_diffrn_reflns_theta_min         2.607
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 'every 50 frames'
_diffrn_standards_number         '2 frames'
_exptl_absorpt_coefficient_mu    1.157
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71012
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
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CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red-purple
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_description       stick
_exptl_crystal_F_000             2816
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.98
_refine_diff_density_min         -1.07
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         3351
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.2630
_refine_ls_R_factor_gt           0.0764
_refine_ls_shift/su_max          0.000162
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
9.12 -10.8 4.16
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0887
_refine_ls_wR_factor_gt          0.0521
_refine_ls_wR_factor_ref         0.0521
_reflns_limit_h_max              21
_reflns_limit_h_min              -21
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              46
_reflns_limit_l_min              0
_reflns_number_gt                3351
_reflns_number_total             18567
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            b704681b.txt
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               7101932