Dehydrohalogenation of proton responsive complexes: versatile aggregation via pyrazolate pincer ligand arms.
Cook, Brian J.; Chen, Chun-Hsing; Pink, Maren; Caulton, Kenneth G.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 2052–2060; doi:10.1039/c7dt04253a

data_7045290
_publ_section_title
;
 Dehydrohalogenation of proton responsive complexes: versatile aggregation
 via pyrazolate pincer ligand arms.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2052
_journal_page_last               2060
_journal_paper_doi               10.1039/c7dt04253a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C138.00 H164 Co5 N30'
_chemical_formula_sum            'C138 H164 Co5 N30'
_chemical_formula_weight         2537.69
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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             14-04-14
_audit_creation_method           CRYSTALS_ver_14.40
_audit_update_record
;
2018-01-05 deposited with the CCDC.
2018-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.412(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   39.4116(19)
_cell_length_b                   16.2047(9)
_cell_length_c                   22.1375(11)
_cell_measurement_reflns_used    9964
_cell_measurement_temperature    150
_cell_measurement_theta_max      14
_cell_measurement_theta_min      3
_cell_volume                     13629.8(12)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_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 0.998
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.053
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12068
_diffrn_reflns_theta_full        25.058
_diffrn_reflns_theta_max         25.058
_diffrn_reflns_theta_min         1.366
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.655
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS, R. Blessing; 1995'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5348.002
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.166
_exptl_crystal_size_min          0.072
_refine_diff_density_max         1.55
_refine_diff_density_min         -0.94
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9681
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     792
_refine_ls_number_reflns         12018
_refine_ls_number_restraints     222
_refine_ls_R_factor_all          0.1044
_refine_ls_R_factor_gt           0.0691
_refine_ls_shift/su_max          0.0496745
_refine_ls_shift/su_mean         0.0011523
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.07P)^2^ +*****P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1863
_refine_ls_wR_factor_gt          0.1708
_refine_ls_wR_factor_ref         0.1863
_reflns_limit_h_max              45
_reflns_limit_h_min              -46
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                8061
_reflns_number_total             12068
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.61
_oxford_diffrn_Wilson_scale      1127.41
_oxford_refine_ls_r_factor_ref   0.1044
_oxford_refine_ls_scale          0.037818(5)
_oxford_reflns_number_all        12018
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title 'mo_14019_0m in C2/c'
_cod_data_source_file            c7dt04253a2.cif
_cod_data_source_block           14019
_cod_depositor_comments
;
The following automatic conversions were performed:

'_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.

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

 Adding full bibliography for 7045287--7045291.cif.
;
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_original_formula_sum        'C138.00 H164 Co5 N30'
_cod_database_code               7045290
_iucr_refine_instruction_details_constraints
;
BLOCK 
CONT SCALE 
CONT CO   (    1 ,X'S,U'S)  UNTIL C    (   12 ) 
CONT C    (   13 ,X'S,U[ISO])  UNTIL C    (   15 ) 
CONT C    (   16 ,X'S,U'S)  UNTIL C    (   54 ) 
CONT C    (   55 ,X'S,U[ISO])  UNTIL C    (  57 ) 
CONT C    (   58 ,X'S,U[ISO])  UNTIL C    (  59 ) 
CONT C    (   60 ,X'S,U'S) 
CONT C    (   61 ,X'S,U[ISO])  UNTIL C    (  63 ) 
CONT C    (   64 ,X'S,U[ISO])  UNTIL C    (  69 ) 
CONT C    (  131 ,X'S,U'S)  UNTIL C    (  571 ) 
CONT C    (  581 ,X'S,U[ISO])  UNTIL C    (  691 ) 
CONT H    (  1 ,X'S) 
SUMFIX PART(1001,OCC) AND PART(1002,OCC) 
SUMFIX PART(1003,OCC) AND PART(1004,OCC) 
SUMFIX PART(1005,OCC) AND PART(1006,OCC) 
SUMFIX PART(1007,OCC) AND PART(1008,OCC) 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) H   ( 132,X'S) H   ( 133,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 142,X'S) H   ( 143,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) H   ( 153,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) H   ( 172,X'S) H   ( 173,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) H   ( 182,X'S) H   ( 183,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) H   ( 192,X'S) H   ( 193,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) H   ( 322,X'S) H   ( 323,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) H   ( 332,X'S) H   ( 333,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 342,X'S) H   ( 343,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 362,X'S) H   ( 363,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) H   ( 372,X'S) H   ( 373,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) H   ( 382,X'S) H   ( 383,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) H   ( 512,X'S) H   ( 513,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) H   ( 522,X'S) H   ( 523,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) H   ( 532,X'S) H   ( 533,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) H   ( 552,X'S) H   ( 553,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) H   ( 562,X'S) H   ( 563,X'S) 
RIDE C   (  57,X'S) H   ( 571,X'S) H   ( 572,X'S) H   ( 573,X'S) 
RIDE C   (  58,X'S) H   ( 581,X'S) 
RIDE C   (  59,X'S) H   ( 591,X'S) 
RIDE C   (  60,X'S) H   ( 601,X'S) 
RIDE C   (  61,X'S) H   ( 611,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) 
RIDE C   (  64,X'S) H   ( 641,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) 
RIDE C   (  67,X'S) H   ( 671,X'S) 
RIDE C   (  68,X'S) H   ( 681,X'S) 
RIDE C   (  69,X'S) H   ( 691,X'S) 
RIDE C   ( 131,X'S) H   (1311,X'S) H   (1312,X'S) H   (1313,X'S) 
RIDE C   ( 141,X'S) H   (1411,X'S) H   (1412,X'S) H   (1413,X'S) 
RIDE C   ( 151,X'S) H   (1511,X'S) H   (1512,X'S) H   (1513,X'S) 
RIDE C   ( 551,X'S) H   (5511,X'S) H   (5512,X'S) H   (5513,X'S) 
RIDE C   ( 561,X'S) H   (5611,X'S) H   (5612,X'S) H   (5613,X'S) 
RIDE C   ( 571,X'S) H   (5711,X'S) H   (5712,X'S) H   (5713,X'S) 
RIDE C   (  581,X'S) H   ( 5811,X'S) 
RIDE C   (  591,X'S) H   ( 5911,X'S) 
RIDE C   (  611,X'S) H   ( 6111,X'S) 
RIDE C   (  621,X'S) H   ( 6211,X'S) 
RIDE C   (  631,X'S) H   ( 6311,X'S) 
RIDE C   ( 641,X'S) H   (6411,X'S) 
RIDE C   ( 671,X'S) H   (6711,X'S) 
RIDE C   ( 681,X'S) H   (6811,X'S) 
RIDE C   ( 691,X'S) H   (6911,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
SAME 0.01, 0.1 FOR 
CONT C(64) C(65) C(66) C(67) C(68) C(69) AND 
CONT C(641) C(65) C(66) C(671) C(681) C(691) AND 
CONT C(64) C(69) C(68) C(67) C(66) C(65) AND 
CONT C(641) C(691) C(681) C(671) C(66) C(65) AND 
CONT C(58) C(59) C(60) C(61) C(62) C(63) AND 
CONT C(60) C(61) C(62) C(63) C(58) C(59) AND 
CONT C(581) C(591) C(60) C(611) C(621) C(631) AND 
CONT C(60) C(611) C(621) C(631) C(581) C(591) 
PLANAR 0.010000  C(58) C(59) C(60) C(61) C(62) C(63) 
SAME 0.01, 0.1 FOR 
CONT C(12) C(1) C(13) C(14) C(15) AND 
CONT C(12) C(1) C(131) C(141) C(151) AND 
CONT C(12) C(1) C(14) C(15) C(13) AND 
CONT C(12) C(1) C(141) C(151) C(131) AND 
CONT C(54) C(49) C(55) C(56) C(57) AND 
CONT C(54) C(49) C(56) C(57) C(55) AND 
CONT C(54) C(49) C(551) C(561) C(571) AND 
CONT C(54) C(49) C(561) C(571) C(551) 
U(IJ)'S  0.0, 0.010000 = C(32) TO C(33) 
U(IJ)'S  0.0, 0.010000 = C(52) TO C(53) 
RESTRAIN 0.0, 0.01=C(15, U[ISO]) - C(13, U[ISO]) 
RESTRAIN 0.0, 0.01=C(34, U[12]) - C(34, U[13]) 
RESTRAIN 0.0, 0.01=C(141, U[22]) - C(141, U[33]) 
RESTRAIN 0.0, 0.01=C(141, U[13]) - C(141, U[23]) 
RESTRAIN 0.0, 0.01=C(551, U[22]) - C(551, U[33]) 
RESTRAIN 0.0, 0.01=C(561, U[22]) - C(561, U[33]) 
RESTRAIN 0.0, 0.01=C(55, U[ISO]) - C(57, U[ISO]) 
RESTRAIN 0.0, 0.01=C(58, U[ISO]) - C(631, U[ISO]) 
RESTRAIN 0.0, 0.01=C(59, U[ISO]) - C(591, U[ISO]) 
RESTRAIN 0.0, 0.01=C(64, U[ISO]) - C(641, U[ISO]) 
RESTRAIN 0.0, 0.01=C(67, U[ISO]) - C(671, U[ISO]) 
RESTRAIN 0.0, 0.01=C(68, U[ISO]) - C(681, U[ISO]) 
RESTRAIN 0.0, 0.01=C(69, U[ISO]) - C(691, U[ISO]) 
U(IJ)'S  0.0, 0.005000 = C(31) TO C(32) 
U(IJ)'S  0.0, 0.005000 = C(31) TO C(34) 
DISTANCE 1.400000 , 0.007000 = C(60) TO C(61) 
DISTANCE 1.400000 , 0.007000 = C(58) TO C(63) 
DISTANCE 1.400000 , 0.007000 = C(581) TO C(631) 
END                                                                             
;