Solid–State Molecular Organometallic Chemistry. Single–Crystal to Single–Crystal Reactivity and Catalysis with Light Hydrocarbon Substrates.
Chadwick, Fredrick M.; McKay, Alasdair I.; Martinez-Martinez, Antonio J.; Rees, Nick; Kraemer, Tobias; Macgregor, Stuart Alan; Weller, Andrew; Chem. Sci.  (2017) –; doi:10.1039/C7SC01491K

data_1546503
_publ_section_title
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 Solid--State Molecular Organometallic Chemistry. Single--Crystal to
 Single--Crystal Reactivity and Catalysis with Light Hydrocarbon
 Substrates.
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_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC01491K
_journal_year                    2017
_chemical_compound_source        SYN
_chemical_formula_moiety         'C32 H12 B F24, C30 H56 P2 Rh'
_chemical_formula_sum            'C62 H68 B F24 P2 Rh'
_chemical_formula_weight         1444.84
_chemical_melting_point          ?
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2015-10-23
_audit_creation_method           CRYSTALS_ver_14.43
_audit_update_record
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2017-03-23 deposited with the CCDC.
2017-07-06 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 90.738(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.2187(18)
_cell_length_b                   17.1982(18)
_cell_length_c                   19.999(3)
_cell_measurement_reflns_used    1672
_cell_measurement_temperature    150
_cell_measurement_theta_max      71
_cell_measurement_theta_min      3
_cell_volume                     6609.7(14)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_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, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.912
_diffrn_measured_fraction_theta_max 0.815
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9108
_diffrn_reflns_theta_full        25.431
_diffrn_reflns_theta_max         74.796
_diffrn_reflns_theta_min         4.081
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.490
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.69
_refine_diff_density_min         -1.04
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9981
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         5511
_refine_ls_number_restraints     102
_refine_ls_R_factor_all          0.1450
_refine_ls_R_factor_gt           0.1072
_refine_ls_shift/su_max          4.7402730
_refine_ls_shift/su_mean         0.1361375
_refine_ls_structure_factor_coef Fsqd
_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: 
 0.358E+04 0.591E+04 0.352E+04 0.136E+04 268. 
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_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3333
_refine_ls_wR_factor_gt          0.2509
_refine_ls_wR_factor_ref         0.3327
_reflns_limit_h_max              23
_reflns_limit_h_min              -23
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                3470
_reflns_number_total             5540
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   4.76
_oxford_diffrn_Wilson_scale      0.82
_oxford_refine_ls_r_factor_ref   0.1449
_oxford_refine_ls_scale          1.373(18)
_oxford_reflns_number_all        5514
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 'C:\Users\ASWGroup\Contacts\Deskt At 11:47 on'
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
EQUIV PART(2002,OCC) PART(2003,OCC) 
WEIGHT -1 PART(2003,OCC) 
END                                                                             
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_iucr_refine_instructions_details_restraints
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NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
DIST 0.0, 0.01 = MEAN  C(1) TO C(2)  C(3) TO C (4) 
DIST 0.0, 0.01 = MEAN  RH(1) TO C(1) RH(1) TO C(2) 
CONT  RH(1) TO C(3) RH(1) TO C(4) 
U(IJ) .0, 0.02000 = C(1) TO C(2) 
U(IJ) .0, 0.02000 = C(3) TO C(4) 
DIST 0.0, 0.01 = MEAN  C(111) TO C (121) C(121) TO C(131) 
CONT C(131) TO C(141) C(141) TO C(151) C(151) TO C(161) 
CONT C(161) TO C(111) C(110) TO C (120) C(120) TO C(130) 
CONT C(130) TO C(140) C(140) TO C(150) C(150) TO C(160) 
CONT C(160) TO C(110) 
U(IJ) .0, 0.02000 = C(111) TO C(121) 
U(IJ) .0, 0.02000 = C(121) TO C(131) 
U(IJ) .0, 0.02000 = C(131) TO C(141) 
U(IJ) .0, 0.02000 = C(141) TO C(151) 
U(IJ) .0, 0.02000 = C(151) TO C(161) 
U(IJ) .0, 0.02000 = C(161) TO C(111) 
U(IJ) .0, 0.02000 = C(110) TO C(120) 
U(IJ) .0, 0.02000 = C(120) TO C(130) 
U(IJ) .0, 0.02000 = C(130) TO C(140) 
U(IJ) .0, 0.02000 = C(140) TO C(150) 
U(IJ) .0, 0.02000 = C(150) TO C(160) 
U(IJ) .0, 0.02000 = C(160) TO C(110) 
END                                                                             
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_cod_data_source_file            c7sc01491k3.cif
_cod_data_source_block           1EthyleneOct
_cod_depositor_comments
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The following automatic conversions were performed:

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

'_atom_sites_solution_primary' value 'Other' changed to 'other'
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.

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

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_original_formula_sum        'C62 H68 B1 F24 P2 Rh1'
_cod_database_code               1546503