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_7045287
_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_absolute_configuration unk
_chemical_formula_moiety         'C111 H149 Co4 N25 O4'
_chemical_formula_sum            'C111 H149 Co4 N25 O4'
_chemical_formula_weight         2133.31
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             14-03-05
_audit_creation_method           CRYSTALS_ver_14.40
_audit_update_record
;
2017-11-09 deposited with the CCDC.
2018-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2926(10)
_cell_length_b                   23.7807(14)
_cell_length_c                   28.6217(16)
_cell_measurement_reflns_used    9682
_cell_measurement_temperature    150
_cell_measurement_theta_max      23
_cell_measurement_theta_min      2
_cell_volume                     11770.1(12)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.971
_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  0.035
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            74359
_diffrn_reflns_theta_full        20.716
_diffrn_reflns_theta_max         23.276
_diffrn_reflns_theta_min         1.113
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.613
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4520
_exptl_crystal_size_max          0.458
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_min          0.128
_refine_diff_density_max         0.83
_refine_diff_density_min         -0.69
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9725
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1236
_refine_ls_number_reflns         15946
_refine_ls_number_restraints     88
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0507
_refine_ls_shift/su_max          0.0185755
_refine_ls_shift/su_mean         0.0010567
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.09P)^2^ +17.30P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1433
_refine_ls_wR_factor_gt          0.1356
_refine_ls_wR_factor_ref         0.1433
_reflns_limit_h_max              19
_reflns_limit_h_min              -19
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                13356
_reflns_number_total             16043
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.70
_oxford_diffrn_Wilson_scale      473.23
_oxford_refine_ls_r_factor_ref   0.0617
_oxford_refine_ls_scale          0.049586(6)
_oxford_reflns_number_all        15946
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title 'mo_14006_0m in P2(1)2(1)2(1)'
_cod_data_source_file            c7dt04253a2.cif
_cod_data_source_block           14006
_cod_depositor_comments
'Adding full bibliography for 7045287--7045291.cif.'
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_database_code               7045287
_iucr_refine_instruction_details_constraints
;
BLOCK 
CONT SCALE 
CONT CO   (    1 ,X'S,U'S)  UNTIL CO   (    4 ) 
CONT O    (    1 ,X'S,U[ISO])  UNTIL O    (   31 ) 
CONT N    (    1 ,X'S,U'S)  UNTIL C    (   12 ) 
CONT C    (   13 ,X'S,U'S)  UNTIL C    (   15 ) 
CONT C    (   16 ,X'S,U'S)  UNTIL C    (   95 ) 
CONT C    (   96 ,X'S,U[ISO])  UNTIL C    (  111 ) 
CONT C    (  131 ,X'S,U'S)  UNTIL C    (  151 ) 
CONT H    (  102 ,X'S)  UNTIL H    (  161 ) 
SUMFIX PART(1001,OCC) AND PART(1002,OCC) 
SUMFIX PART(1003,OCC) AND PART(1004,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   (  59,X'S) H   ( 591,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   (  67,X'S) H   ( 671,X'S) 
RIDE C   (  70,X'S) H   ( 701,X'S) H   ( 702,X'S) H   ( 703,X'S) 
RIDE C   (  71,X'S) H   ( 711,X'S) H   ( 712,X'S) H   ( 713,X'S) 
RIDE C   (  72,X'S) H   ( 721,X'S) H   ( 722,X'S) H   ( 723,X'S) 
RIDE C   (  74,X'S) H   ( 741,X'S) H   ( 742,X'S) H   ( 743,X'S) 
RIDE C   (  75,X'S) H   ( 751,X'S) H   ( 752,X'S) H   ( 753,X'S) 
RIDE C   (  76,X'S) H   ( 761,X'S) H   ( 762,X'S) H   ( 763,X'S) 
RIDE C   (  78,X'S) H   ( 781,X'S) 
RIDE C   (  81,X'S) H   ( 811,X'S) 
RIDE C   (  82,X'S) H   ( 821,X'S) 
RIDE C   (  83,X'S) H   ( 831,X'S) 
RIDE C   (  86,X'S) H   ( 861,X'S) 
RIDE C   (  89,X'S) H   ( 891,X'S) H   ( 892,X'S) H   ( 893,X'S) 
RIDE C   (  90,X'S) H   ( 901,X'S) H   ( 902,X'S) H   ( 903,X'S) 
RIDE C   (  91,X'S) H   ( 911,X'S) H   ( 912,X'S) H   ( 913,X'S) 
RIDE C   (  93,X'S) H   ( 931,X'S) H   ( 932,X'S) H   ( 933,X'S) 
RIDE C   (  94,X'S) H   ( 941,X'S) H   ( 942,X'S) H   ( 943,X'S) 
RIDE C   (  95,X'S) H   ( 951,X'S) H   ( 952,X'S) H   ( 953,X'S) 
RIDE C   (  96,X'S) H   ( 961,X'S) H   ( 962,X'S) 
RIDE C   (  97,X'S) H   ( 971,X'S) H   ( 972,X'S) 
RIDE C   (  98,X'S) H   ( 981,X'S) H   ( 982,X'S) 
RIDE C   (  99,X'S) H   ( 991,X'S) H   ( 992,X'S) 
RIDE C   ( 100,X'S) H   (1001,X'S) H   (1002,X'S) 
RIDE C   ( 101,X'S) H   (1011,X'S) H   (1012,X'S) 
RIDE C   ( 102,X'S) H   (1021,X'S) H   (1022,X'S) 
RIDE C   ( 103,X'S) H   (1031,X'S) H   (1032,X'S) 
RIDE C   ( 104,X'S) H   (1041,X'S) H   (1042,X'S) 
RIDE C   ( 105,X'S) H   (1051,X'S) H   (1052,X'S) 
RIDE C   ( 106,X'S) H   (1061,X'S) H   (1062,X'S) 
RIDE C   ( 107,X'S) H   (1071,X'S) H   (1072,X'S) 
RIDE C   ( 108,X'S) H   (1081,X'S) H   (1082,X'S) 
RIDE C   ( 109,X'S) H   (1091,X'S) H   (1092,X'S) 
RIDE C   ( 110,X'S) H   (1101,X'S) H   (1102,X'S) 
RIDE C   ( 111,X'S) H   (1111,X'S) H   (1112,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) 
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(105) O(3) C(107) AND 
CONT C(107) O(3) C(105) AND 
CONT C(105) O(31) C(107) AND 
CONT C(107) O(31) C(105) 
SAME 0.01, 0.1 FOR 
CONT C(12) C(1) C(13) C(14) C(15) AND 
CONT C(12) C(1) C(14) C(15) C(13) AND 
CONT C(12) C(1) C(131) C(141) C(151) AND 
CONT C(12) C(1) C(141) C(151) C(131) 
RESTRAIN 0.0, 0.001 = O(3,U[ISO]) - O(31,U[ISO]) 
RESTRAIN 0.0, 0.001 = C(104,U[ISO]) - C(105,U[ISO]) 
RESTRAIN 0.0, 0.001 = C(14,U[11]) - C(14,U[22]) 
RESTRAIN 0.0, 0.001 = C(97,U[ISO]) - C(98,U[ISO]) 
DISTANCE 1.450000 , 0.005000 = O(3) TO C(107) 
U(IJ)'S  0.0, 0.005000 = C(12) TO C(13) 
U(IJ)'S  0.0, 0.005000 = C(12) TO C(14) 
U(IJ)'S  0.0, 0.005000 = C(13) TO C(15) 
U(IJ)'S  0.0, 0.005000 = C(15) TO C(151) 
U(IJ)'S  0.0, 0.005000 = C(13) TO C(131) 
RESTRAIN 0.0, 0.001 = C(110,U[ISO]) - C(111,U[ISO]) 
END                                                                             
;