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_1546505
_publ_section_title
;
 Solid--State Molecular Organometallic Chemistry. Single--Crystal to
 Single--Crystal Reactivity and Catalysis with Light Hydrocarbon
 Substrates.
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC01491K
_journal_year                    2017
_chemical_absolute_configuration ad
_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           182
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 6c 2c'
_symmetry_space_group_name_H-M   'P 63 2 2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2016-01-25
_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.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   25.8617(3)
_cell_length_b                   25.8617(3)
_cell_length_c                   20.3020(3)
_cell_measurement_reflns_used    18965
_cell_measurement_temperature    150
_cell_measurement_theta_max      76
_cell_measurement_theta_min      4
_cell_volume                     11759.4(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.992
_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  0.121
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            83387
_diffrn_reflns_theta_full        75.081
_diffrn_reflns_theta_max         76.614
_diffrn_reflns_theta_min         2.938
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.943
_exptl_absorpt_correction_T_max  0.56
_exptl_absorpt_correction_T_min  0.29
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4416
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.05
_refine_diff_density_min         -0.77
_refine_ls_abs_structure_details 'Flack (1983), 541 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.009(16)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9722
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         8174
_refine_ls_number_restraints     456
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0666
_refine_ls_shift/su_max          0.0099694
_refine_ls_shift/su_mean         0.0002300
_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: 
 0.247E+04 0.407E+04 0.262E+04 0.119E+04 314. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2106
_refine_ls_wR_factor_gt          0.1776
_refine_ls_wR_factor_ref         0.2105
_reflns_limit_h_max              0
_reflns_limit_h_min              -27
_reflns_limit_k_max              32
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                6250
_reflns_number_total             8209
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.15
_oxford_diffrn_Wilson_scale      0.52
_oxford_refine_ls_r_factor_ref   0.0868
_oxford_refine_ls_scale          1.545(11)
_oxford_reflns_number_all        8175
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title
'C:\Users\ASWGroup\Contacts\Deskt At 11:37 on'
_cod_data_source_file            c7sc01491k3.cif
_cod_data_source_block           1EthyleneHex
_cod_depositor_comments
;
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      'P 63 2 2 '
_cod_original_formula_sum        'C62 H68 B1 F24 P2 Rh1'
_cod_database_code               1546505
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
CONT ENANTIO 
RIDE C   (   1,X'S) H   (  12,X'S) H   (  11,X'S) 
RIDE C   (   2,X'S) H   (  22,X'S) H   (  21,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) H   (  42,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) H   (  52,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) H   (  62,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) H   (  72,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) H   (  82,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) H   ( 102,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) H   ( 112,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) H   ( 122,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) H   ( 132,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 142,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
EQUIV PART(2001,OCC) PART(2002,OCC) 
WEIGHT -1 PART(2002,OCC) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
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NO 
SAME C(28) C(31) F(101) F(111) F(120) AND 
CONT C(28) C(31) F(111) F(120) F(101) AND 
CONT C(28) C(31) F(120) F(101) F(111) AND 
CONT C(28) C(31) F(100) F(110) F(121) AND 
CONT C(28) C(31) F(110) F(121) F(100) AND 
CONT C(28) C(31) F(121) F(100) F(110) 
DELU 0.015 C(28) C(31) F(101) F(111) F(120) AND 
CONT C(28) C(31) F(111) F(120) F(101) AND 
CONT C(28) C(31) F(120) F(101) F(111) AND 
CONT C(28) C(31) F(100) F(110) F(121) AND 
CONT C(28) C(31) F(110) F(121) F(100) AND 
CONT C(28) C(31) F(121) F(100) F(110) 
SIMU 0.015 C(28) C(31) F(101) F(111) F(120) AND 
CONT C(28) C(31) F(111) F(120) F(101) AND 
CONT C(28) C(31) F(120) F(101) F(111) AND 
CONT C(28) C(31) F(100) F(110) F(121) AND 
CONT C(28) C(31) F(110) F(121) F(100) AND 
CONT C(28) C(31) F(121) F(100) F(110) 
SAME C(18) C(22) F(11) F(20) F(30) AND 
CONT C(18) C(22) F(20) F(30) F(11) AND 
CONT C(18) C(22) F(30) F(11) F(20) AND 
CONT C(18) C(22) F(10) F(21) F(31) AND 
CONT C(18) C(22) F(21) F(31) F(10) AND 
CONT C(18) C(22) F(31) F(10) F(21) 
DELU 0.015 C(18) C(22) F(11) F(20) F(30) AND 
CONT C(18) C(22) F(20) F(30) F(11) AND 
CONT C(18) C(22) F(30) F(11) F(20) AND 
CONT C(18) C(22) F(10) F(21) F(31) AND 
CONT C(18) C(22) F(21) F(31) F(10) AND 
CONT C(18) C(22) F(31) F(10) F(21) 
SIMU 0.015 C(18) C(22) F(11) F(20) F(30) AND 
CONT C(18) C(22) F(20) F(30) F(11) AND 
CONT C(18) C(22) F(30) F(11) F(20) AND 
CONT C(18) C(22) F(10) F(21) F(31) AND 
CONT C(18) C(22) F(21) F(31) F(10) AND 
CONT C(18) C(22) F(31) F(10) F(21) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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