Structural diversity of ethylzinc derivatives of 3,5-substituted pyrazoles.
Komorski, Szymon; Leszczyński, Michał K; Justyniak, Iwona; Lewiński, Janusz; Dalton transactions (Cambridge, England : 2003) 49 (2020) 17388–17394; doi:10.1039/d0dt03026k

data_7706107
_publ_section_title
;
 Structural diversity of ethylzinc derivatives of 3,5-substituted
 pyrazoles.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17388
_journal_page_last               17394
_journal_paper_doi               10.1039/d0dt03026k
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C26 H36 N4 O2 Zn2'
_chemical_formula_sum            'C26 H36 N4 O2 Zn2'
_chemical_formula_weight         567.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_Int_Tables_number      15
_audit_creation_date             2020-08-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-08-24 deposited with the CCDC.	2020-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.417(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2907(9)
_cell_length_b                   16.3872(10)
_cell_length_c                   13.4133(11)
_cell_measurement_reflns_used    1978
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      28.0220
_cell_measurement_theta_min      3.5310
_cell_volume                     2547.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2974
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9835
_diffrn_measured_fraction_theta_max 0.9835
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      7.00  77.00   1.00   90.00    --   27.49  57.00 -30.00   70
  2  \w     43.00  84.00   1.00   90.00    --   27.49-119.00  91.00   41
  3  \w     12.00  88.00   1.00   90.00    --   27.49  77.00 150.00   76
  4  \w    -45.00  46.00   1.00   90.00    --   27.49 -77.00  30.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0303894000
_diffrn_orient_matrix_UB_12      -0.0298989000
_diffrn_orient_matrix_UB_13      -0.0185263000
_diffrn_orient_matrix_UB_21      -0.0208309000
_diffrn_orient_matrix_UB_22      -0.0307902000
_diffrn_orient_matrix_UB_23      0.0261196000
_diffrn_orient_matrix_UB_31      -0.0488859000
_diffrn_orient_matrix_UB_32      -0.0054432000
_diffrn_orient_matrix_UB_33      -0.0460527000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5259
_diffrn_reflns_theta_full        26.9978
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         3.22
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.913
_exptl_absorpt_correction_T_max  0.795
_exptl_absorpt_correction_T_min  0.582
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.4790
_exptl_crystal_description       plate
_exptl_crystal_F_000             1186.8169
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.5187
_refine_diff_density_min         -0.8272
_refine_diff_density_rms         0.1324
_refine_ls_d_res_high            0.7828
_refine_ls_d_res_low             6.3252
_refine_ls_goodness_of_fit_ref   1.0447
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    29
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2737
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0447
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1008P)^2^+0.4170P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1447
_refine_ls_wR_factor_ref         0.1602
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -15
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                2281
_reflns_number_total             2737
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0dt03026k2.cif
_cod_data_source_block           nowa
_cod_database_code               7706107
_chemical_oxdiff_formula         'C40 H30 N4 O4 Zn2'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C3(H3a,H3b), C4(H4a,H4b), C5(H5a,H5b), C6(H6a,H6b)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C10(H10), C11(H11), C12(H12)
2.c Idealised Me refined as rotating group:
 C2(H2a,H2b,H2c)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.911
_oxdiff_exptl_absorpt_empirical_full_min 0.479